Microwave reaction synthesis method for endogenous metal matrix composite material

A composite material and microwave reaction technology, applied in the field of microwave reaction synthesis method, to achieve the effect of purifying the matrix, shortening the preparation cycle, and refining the structure

Inactive Publication Date: 2010-03-10

NANJING UNIV OF SCI & TECH

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AI-Extracted Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a microwave reaction method for endogenous metal matrix composites that is simple in process operation, safe and reliable, ener...

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Method used

(2) loading compacted sample is inserted into reaction unit, see Fig. 1; Note following points when loading sample: 1) expose the top of compacted sample, to guarantee the accurate of sample top infrared temperature measurement 2) SiC wave absorbing agent should not block the monitoring hole on the side, so as to ensure the color change in the top chamber of the sample observed from the side during the reaction process; 3) SiC wave absorbing agent should not be compacted, so as to ensure that the wave absorbing agent reacts in the sample. 4) The height of the sample can be adjusted through the high alumina foam brick at the bottom of the sample to ensure that the top of the sample is basically flush with the side observation hole for easy observation;

(2) loading compacted sample is inserted reaction unit, see Fig. 1; Note following points when loading sample: 1) the top of exposed compacted sample, to guarantee the accurate of sample top infrared temperature measurement 2) SiC wave absorbing agent should not block the monitoring hole on the side, so as to ensure the color change in the top chamber of the sample observed from the side during the reaction process; 3) SiC wave absorbing agent should not be compacted, so as to ensure that the wave absorbing agent reacts in the sample. 4) The height of the sample can be adjusted through the high alumina foam brick at the bottom of the sample to ensure that the top of the sample is basically flush with the side observation hole for easy observation;

(2) loading compacted sample is put into reaction unit (see Fig. 1); Pay attention to following points when loading sample: 1) expose the top of compacted sample, to guarantee the infrared temperature measurement of sample top Accuracy; 2) SiC wave absorbing agent should not block the monitoring hole on the side to ensure that the color change in the top cavity of the sample is observed from the side during the reaction process; ...

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Abstract

The invention discloses a microwave reaction synthesis method for an endogenous metal matrix composite material, which comprises the following steps: preparing a reaction sample; filling the sample, namely filling the pressed sample into a reaction device, and filling an SiC wave-absorbing agent around the sample; pumping vacuum; synthesizing microwave, namely regulating microwave input power to alower limit value, closing a gate and powering on the sample; preserving heat, namely when the color of the reaction sample is suddenly changed and simultaneously the temperature change curve recorded by far infrared rays is hastily raised to produce sharp steep peaks, reducing the microwave input power to preserve the heat, and stopping microwave input after the heat is preserved for a certain time; and discharging the sample from a furnace, namely after a vacuum furnace is cooled, taking the reaction device out, and taking the reaction sample out from the reaction device to obtain the endogenous composite material. The microwave reaction synthesis method has the advantages of simple process operation, safety and reliability, energy conservation and time saving, environmental protectionand simplified operation process, can greatly reduce the energy consumption, saves the energy as high as 70 to 90 percent, and shortens the preparation period which is generally about 15 minutes.

Technology Topic

Vacuum furnacePumping vacuum +9

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Examples

Experimental program(4)

Example Embodiment

[0027] Example 1: Al-TiO 2 -B reaction system

[0028] (1) Prepare the reaction sample with Al, TiO 2 , B powder according to the set reinforcement (TiB 2 And Al 2 O 3 ) Volume fraction (such as 30%), from the chemical reaction formula: 4Al+3TiO 2 +6B→3TiB 2 +2Al 2 O 3 By stoichiometric calculation, the reaction formula Meet the thermodynamic conditions of the reaction. It is calculated that 20g reaction sample requires 15.43g Al powder and TiO 2 Powder 4.57g and B powder 0.57g. Then put it in a ball mill tank, mix it with a ball mill at a ball-to-powder ratio of 5:1 and a rotation speed of 300p.r.m, and then extrude it at a pressure of 120MPa to form a compact sample;

[0029] (2) Sample loading Put the compact sample into the reaction device, see figure 1; Pay attention to the following points when loading samples: 1) Bare the top of the compact sample to ensure the accuracy of infrared temperature measurement on the top of the sample; 2) Do not block the side monitoring hole with SiC absorber to ensure the side during the reaction Observe the color change in the cavity at the top of the sample; 3) Do not compact the SiC absorber to ensure that the absorber does not agglomerate after the sample is reacted and can be reused; 4) The height of the sample can pass the height of the bottom of the sample Aluminum foam bricks are used to adjust to ensure that the top of the sample is basically flush with the side observation hole for observation;

[0030] (3) Vacuum the reaction device into a vacuum microwave oven (3kW), vacuum to 10 -4 -10 -3;

[0031] (4) Microwave synthesis adjust the microwave input power. When the microwave acts for about 5 minutes, the compact sample undergoes a chemical reaction. At this time, it can be seen through the observation hole that the color of the reaction sample gradually turns red and instantly turns white. The chemical reaction was violent, and the temperature curve of the reaction sample recorded by the infrared detection device also showed a steep rise.

[0032] (5) Heat preservation Once the reaction sample undergoes a chemical reaction, the microwave input power can be reduced to 0.5 kW to continue working, and the microwave input should be stopped after about 10 minutes.

[0033] (6) Cooling out of the furnace and opening the furnace after cooling for 10 minutes, and sampling after air cooling.

[0034] The preparation cycle of the reaction system is about 30 minutes. After the reaction, the structure of the composite material is fine, and the reinforcement is (Al 2 O 3 +TiB 2 ), compared with the composite material synthesized by traditional heating reaction, the distribution uniformity and compactness of the structure are significantly improved, and there are no holes, see figure 2.

Example Embodiment

[0035] Example 2: Al-ZrO 2 system

[0036] (1) Prepare the reaction sample by Al, ZrO 2 Powder according to the set reinforcement (Al 3 Zr and Al 2 O 3 ) Volume fraction (such as 30%), from the chemical reaction formula: 13Al+3ZrO 2 →3Al 3 Zr+2Al 2 O 3 By stoichiometric calculation, the reaction formula Meet the thermodynamic conditions of the reaction. By calculation, a 20g reaction sample requires 16.1g Al powder and ZrO 2 3.9g powder, then put it into a ball mill tank, mix it with a ball mill at a ball-to-powder ratio of 5:1 and a rotation speed of 300p.r.m, and then extrude it at a pressure of 120MPa to form a compact sample;

[0037] (2) Sample loading Put the compact sample into the reaction device, see figure 1; Pay attention to the following points when loading samples: 1) Bare the top of the compact sample to ensure the accuracy of infrared temperature measurement on the top of the sample; 2) Do not block the side monitoring hole with SiC absorber to ensure the side during the reaction Observe the color change in the cavity at the top of the sample; 3) Do not compact the SiC absorber to ensure that the absorber does not agglomerate after the sample is reacted and can be reused; 4) The height of the sample can pass the height of the bottom of the sample Aluminum foam bricks are used to adjust to ensure that the top of the sample is basically flush with the side observation hole for observation;

[0038] (3) Vacuum the reaction device into a vacuum microwave oven (3kW), vacuum to 10 -4 -10 -3;

[0039] (4) Microwave synthesis adjust the microwave input power. When the microwave is applied for 5-6 minutes, the compact sample undergoes a chemical reaction. At this time, it can be seen through the observation hole that the color of the reaction sample gradually turns red and instantly turns white. A violent chemical reaction occurred, and the temperature curve of the reaction sample recorded by the infrared detection device also showed a steep rise.

[0040] (5) Heat preservation Once the reaction sample undergoes a chemical reaction, the microwave input power can be appropriately lowered, such as 0.5kW and continue to work, after about 12 minutes, stop the microwave input.

[0041] (6) After cooling down the furnace, the furnace will be turned on after 14 minutes of cooling, and the sample will be taken after air cooling.

[0042] The preparation cycle of the reaction system is about 30 minutes. After the reaction, the structure of the composite material is fine, and the reinforcement is (Al 2 O 3 +ZrAl 3 ), compared with the composite material synthesized by traditional heating reaction, the distribution uniformity and compactness of the structure are significantly improved, see image 3.

Example Embodiment

[0043] Example 3: Al-Ni 2 O 3 reaction system

[0044] (1) Prepare the reaction sample by combining Al and Ni 2 O 3 Powder according to the set reinforcement (Ni 2 Al 3 And Al 2 O 3 ) Volume fraction (such as 20%), from the chemical reaction formula: 5Al+Ni 2 O 3 →Ni 2 Al 3 +Al 2 O 3 By stoichiometric calculation, the reaction formula Meet the thermodynamic conditions of the reaction. It is calculated that 20g reaction sample requires 13.26g Al powder and Ni 2 O 3 1.74g powder, then put it into a ball mill tank, mix it with a ball mill at a ball-to-powder ratio of 5:1 and a rotation speed of 300p.r.m, and then extrude into a billet at a pressure of 120MPa to make a compact sample;

[0045] (2) Sample loading Place the compact sample into the reaction device (see figure 1 ); Pay attention to the following points when loading the sample: 1) Bare the top of the compact sample to ensure the accuracy of infrared temperature measurement on the top of the sample; 2) Do not block the side monitoring hole with SiC absorber to ensure the reaction process Observe the color change in the cavity at the top of the sample from the side; 3) Do not compact the SiC absorber to ensure that the absorber does not agglomerate after the reaction of the sample and can be reused; 4) The height of the sample can pass through the bottom of the sample The high-aluminum foam bricks are adjusted to ensure that the top of the sample is basically flush with the side observation hole for easy observation;

[0046] (3) Vacuum the reaction device into a vacuum microwave oven (3kW), vacuum to 10 -4 -10 -3;

[0047] (4) Microwave synthesis adjust the microwave input power. When the microwave acts on for about 1 minute, the compact sample undergoes a chemical reaction. At this time, it can be seen through the observation hole that the color of the reaction sample gradually turns red and instantly turns white. An extremely violent chemical reaction took place, and the temperature curve of the reaction sample recorded by the infrared detection device also showed a steep rise.

[0048] (5) Heat preservation Once the reaction sample undergoes a chemical reaction, the microwave input power can be moderately reduced, such as 0.5kW to continue to work, about 15 minutes later, stop the microwave input.

[0049] (6) Let the furnace cool down and start the furnace after 15 minutes of cooling, and take samples after air cooling.

[0050] The preparation cycle of the reaction system is about 20 minutes. After the reaction, the structure of the composite material is fine, and the reinforcement is (Ni 2 Al 3 +Al 2 O 3 ), see its organization Figure 4 , The thick rod structure in the picture is Ni 2 Al 3 , Al 2 O 3 It is a fine particle, due to its poor wettability with the Al matrix, it is difficult to enter the Al matrix and become a nucleus when the matrix solidifies and crystallize, and is distributed in the grain boundaries of the particles.

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Classification and recommendation of technical efficacy words

The operation process is simple
Simple process operation

Microwave reaction synthesis method for endogenous metal matrix composite material

A composite material and microwave reaction technology, applied in the field of microwave reaction synthesis method, to achieve the effect of purifying the matrix, shortening the preparation cycle, and refining the structure

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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