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CN109865831B - A kind of degassing method of particle reinforced aluminum matrix composite powder - Google Patents

A kind of degassing method of particle reinforced aluminum matrix composite powder Download PDF

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CN109865831B
CN109865831B CN201711265812.9A CN201711265812A CN109865831B CN 109865831 B CN109865831 B CN 109865831B CN 201711265812 A CN201711265812 A CN 201711265812A CN 109865831 B CN109865831 B CN 109865831B
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vacuum
vacuum valve
decompression chamber
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CN109865831A (en
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左涛
聂俊辉
刘彦强
杨必成
马自力
樊建中
魏少华
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Youyan Metal Composite Materials (Beijing) Co.,Ltd.
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GRIMN Engineering Technology Research Institute Co Ltd
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Abstract

本发明公开了一种低粉末损耗、低真空波动的颗粒增强铝基复合材料粉末的除气方法,该方法包括如下步骤:将复合材料粉末装入包套中;在复合材料粉末上表面覆盖带有孔洞的遮挡铝箔,焊好带有抽气管的包套上盖;将包套放入加热炉内,连接可控减压舱及真空机组;启动真空机组,打开减压舱与真空机组之间的真空阀B,当减压舱内真空度达到1×10‑2Pa‑9900Pa后,关闭真空阀B,打开连接包套抽气管的真空阀A,至数字真空计示数基本稳定后,关闭真空阀A,完成一次包套减压操作;经数次减压操作,打开真空阀A和真空阀B,加热包套;在波动温度点保温,待真空波动消失后继续加热;加热及保温过程结束,关闭真空阀,封死抽气管,完成真空除气过程。

Figure 201711265812

The invention discloses a degassing method for particle-reinforced aluminum-based composite material powder with low powder loss and low vacuum fluctuation. The method comprises the steps of: packing the composite material powder into a package; covering the upper surface of the composite material powder with a tape Cover the aluminum foil with holes, and weld the upper cover of the package with the exhaust pipe; put the package into the heating furnace, connect the controllable decompression chamber and the vacuum unit; start the vacuum unit and open the space between the decompression chamber and the vacuum unit When the vacuum degree in the decompression chamber reaches 1× 10-2 Pa-9900Pa, close the vacuum valve B, open the vacuum valve A connected to the exhaust pipe of the package, and close the digital vacuum gauge after the reading is basically stable. Vacuum valve A, complete a decompression operation of the envelope; after several decompression operations, open the vacuum valve A and vacuum valve B to heat the envelope; keep warm at the fluctuating temperature point, and continue heating after the vacuum fluctuation disappears; the heating and heat preservation process At the end, close the vacuum valve, seal the exhaust pipe, and complete the vacuum degassing process.

Figure 201711265812

Description

Degassing method of particle-reinforced aluminum-based composite material powder
Technical Field
The invention relates to a degassing method of particle reinforced aluminum matrix composite powder, in particular to a degassing treatment method of powder metallurgy particle reinforced aluminum matrix composite powder by using a controllable decompression chamber.
Background
Compared with other light materials such as aluminum and magnesium alloy, the particle reinforced aluminum matrix composite material generally has the outstanding advantages of high specific strength, high specific stiffness, fatigue resistance, low expansion coefficient and the like, and particularly has certain designability of material performance. Through research and development in recent ten years in China, application breakthroughs are obtained in the fields of aerospace, military industry and the like, and the method has wide development prospects in the future.
At present, the main preparation methods of the particle reinforced aluminum matrix composite material comprise: powder metallurgy, stirring fusion casting, rapid cold deposition, pressure casting, etc. The powder metallurgy method has the advantages of easy design of the type, granularity, content and distribution of the reinforcement, easy control of the combination condition of the matrix and the reinforced interphase interface, good reproducibility of material performance and the like, and becomes a preparation technical route which is mainly developed.
The general production flow of preparing the particle reinforced aluminum matrix composite material by the powder metallurgy method comprises the following steps: the method comprises the steps of raw material powder pretreatment, powder mixing and canning, vacuum degassing, hot forming and subsequent machining. The present invention is concerned with vacuum degassing processes. Vacuum degassing is a technological process of loading composite material mixed powder into a sealed sheath with an exhaust pipe, connecting a vacuum unit, reaching a corresponding vacuum degree at a certain temperature, preserving heat for a period of time, and then sealing the exhaust pipe. In the prior art, two problems exist:
firstly, there is partial powder to pass through the exhaust tube suction vacuum unit inner chamber, has increased the combined material and has mixed the powder loss to shorten the working life of vacuum unit, increased product manufacturing cost on the whole.
And secondly, during large-scale production, a plurality of vacuum units are connected with a plurality of bags one by one and are sleeved in a heating furnace for heating treatment. In the heating and heat preservation processes, the powder in each sheath has an air release phenomenon, the specific air release amount naturally fluctuates due to different specific conditions (relative density fluctuation, powder weight fluctuation and the like), and the air exhaust capacities of the vacuum units connected one by one in each sheath are different, so that the vacuum fluctuation in the sheath is caused. The process requires that the temperature is kept for a certain time at a fluctuation temperature point, and the heating is continued after the vacuum fluctuation disappears. Therefore, the vacuum fluctuation prolongs the process time, reduces the production efficiency of the product and increases the production cost of the product.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a degassing method for particle-reinforced aluminum-based composite powder, which utilizes a controllable decompression chamber and a shielding aluminum foil to realize vacuum degassing of the particle-reinforced aluminum-based composite powder with low powder loss and low vacuum fluctuation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of degassing a particle-reinforced aluminium-based composite powder, the method comprising the steps of:
(1) filling the mixed particle reinforced aluminum-based composite material powder into a sheath, and vibrating or tamping the powder to ensure that the apparent density of the powder is 50-70% of the theoretical density;
(2) covering a shielding aluminum foil on the upper surface of the composite material powder, drilling a plurality of holes at random positions on the shielding aluminum foil, and welding a sheath upper cover with an exhaust tube;
(3) placing the sheath filled with the composite material powder into a heating furnace, and connecting the sheath with an air inlet of a controllable decompression chamber through an exhaust tube, a vacuum hose and a vacuum valve A; a digital vacuum gauge capable of displaying the pressure in the controllable decompression chamber is arranged on the controllable decompression chamber; the air outlet of the controllable decompression chamber is connected with a vacuum unit through a vacuum valve B;
(4) starting the vacuum unit, opening the vacuum valve B, observing the number of the digital vacuum meter, and when the number reaches 1 × 10-2After Pa-9900Pa, closing the vacuum valve B, opening the vacuum valve A connected with the sheath exhaust pipe, and closing the vacuum valve A to finish one sheath pressure reduction operation after the reading of the digital vacuum meter is basically stable;
(5) after several times of decompression operation, the vacuum degree of the decompression chamber and the sheath can reach 1-9 x 10-2Pa, opening a vacuum valve A and a vacuum valve B, and starting heating the sheath; in the heating process, the sheath is deflated, the fluctuation of the vacuum degree occurs, the temperature is preserved at the fluctuation temperature point, and the heating is continued after the vacuum fluctuation disappears;
(6) and (5) closing the vacuum valve A and the vacuum valve B after the heating and heat preservation process is finished, sealing the exhaust pipe, taking the sheath out of the heating furnace, and finishing the vacuum degassing process.
In the step (1), the overall dimension of the sheath is determined by the size of a billet required by the process, and the sheath is generally made of industrial pure aluminum through welding.
In the step (2), the shielding aluminum foil is industrial pure aluminum, the thickness of the shielding aluminum foil is 0.5-5mm, and the size of the shielding aluminum foil is slightly smaller than the inner diameter of the sheath in the step (1). The shielding aluminum foil has the function of increasing the gas extraction resistance in the sheath, is favorable for reducing the gas extraction force and is favorable for reducing the powder loss. Covering 1-10 layers of shielding aluminum foils on the upper surface of the composite material powder, wherein the thickness of each layer of shielding aluminum foil is 0.5-5mm, and holes with the diameter of 0.1-0.5mm are punched at 3-10 random positions on the shielding aluminum foil.
In the step (3), the controllable decompression chamber is a stainless steel pressure-resistant shell, the volume of the controllable decompression chamber is 2 times larger than the sum of the volumes of the jackets to be treated, and the inner surface of the controllable decompression chamber is polished. And both ends of the controllable decompression chamber are respectively provided with an air outlet and an air inlet. The diameter of the air outlet is close to the working diameter of the diffusion pump of the vacuum unit, the number of the air outlet is the same as that of the vacuum units, and the position of the air outlet is higher than that of the air inlet; the diameter of the air inlets is between 20 and 60mm, and the number of the air inlets is equal to the number of the jackets to be treated. The controllable decompression chamber is provided with a digital vacuum gauge, and the measurement range is from normal pressure to 1 multiplied by 10-5Pa, measurement accuracy. + -. 1% reading. The vacuum valve A, B, the vacuum hose and the like are commercially available and can meet the vacuum sealing requirements of the process.
And (4) substantially pumping the controllable decompression chamber to a certain vacuum degree by using a vacuum unit, and communicating the controllable decompression chamber with the sheath to be treated to realize decompression operation inside the sheath. Through theoretical analysis and experiments, the important relevant factor of the powder loss is the pressure difference between the internal pressure of the sheath and the air inlet of the vacuum unit, the larger the pressure difference is, the larger the powder loss is, the smaller the pressure difference is, and the smaller the powder loss is. The process means for controlling the air exhaust pressure difference is provided by utilizing the controllable decompression chamber to decompress the sheath, so that the optimum process combination with low air exhaust powder loss and high decompression efficiency can be found out through tests aiming at specific products.
In the step (5), the sheath is vacuumized to 1-9 x 10 by a vacuum unit and a controllable decompression chamber-2After Pa, the sheath is not decompressed by the controllable decompression chamber, but the sheath is directly vacuumized by a vacuum unit through the space of the decompression chamber. This is because it has been found in practice that the loss of powder during the evacuation process occurs substantially when the vacuum in the jacket decreases from atmospheric pressure to 1X 10-1During Pa, the vacuum degree of the sheath reaches 1X 10-2-9×10-2After Pa, almost no powder loss occurred. Therefore, in order to improve the air extraction efficiency, the decompression chamber is not used for sheath decompression.
And (5) in the process of exhausting, heating and preserving heat of the sheath in the step (5), the billet ingot in the sheath can have an air release phenomenon, so that the vacuum degree in the sheath fluctuates. The production process of the product needs to keep the temperature for a certain time at the fluctuation temperature point, and then the heating is continued after the vacuum fluctuation disappears. In the new process with the controllable decompression chamber, because all the vacuum units are connected with the controllable decompression chamber, the fluctuation of the air pumping capacity of different vacuum units can be overcome; the controllable decompression chamber is connected with all the sheaths, and the volume of the controllable decompression chamber is far larger than that of each sheath, so that the vacuum fluctuation in the sheaths can be effectively reduced, the heat preservation time of a fluctuation temperature point is shortened, the vacuum degassing efficiency is improved, and the production cost of products is further reduced.
The invention has the advantages that:
1. by using the controllable decompression chamber and the shielding aluminum foil, the air suction strength of the vacuum unit to the sheath can be controlled. Through process tests, the optimal process combination of low powder loss and high air extraction efficiency can be found, the powder loss is greatly reduced, and the production cost of powder products is reduced.
2. By using the decompression chamber with a controllable certain volume, the vacuum unit and the ladle sleeve to be treated are connected together, so that the vacuum fluctuation in the ladle sleeve in the technical process is effectively reduced, the technical time is shortened, the vacuum degassing efficiency is improved, and the production cost of products is further reduced.
3. By using the controllable decompression chamber and the shielding aluminum foil, the quantity of product powder entering the vacuum unit in the air exhaust process is reduced, the service life of the vacuum unit is prolonged, and the production cost of the product is reduced.
By adopting the innovative vacuum degassing method, the loss of product powder in the process is reduced, the vacuum fluctuation in the process is reduced, the process time is shortened, and the product production cost is reduced.
Drawings
FIG. 1 is a schematic cross-sectional view of a to-be-treated wrap equipped with a shielding aluminum foil.
FIG. 2 is a top view of the connection of the controllable vacuum chamber to the vacuum unit and jacket.
Reference numerals:
heating furnace with 1. 2 cases of composite powder, 3 cases of shielding aluminum foil, 4 cases of covering and 11. covering
12 vacuum hose 13 vacuum valve a 14 decompression chamber air inlet 15 controllable decompression chamber
16 decompression chamber air outlet 17 vacuum valve B18 vacuum unit 19 digital vacuum gauge
Detailed Description
The invention is further illustrated by the following examples and figures, which are not meant to limit the scope of the invention.
As shown in figures 1 and 2, the invention utilizes the controllable decompression chamber to carry out the degassing treatment of the powder metallurgy particle reinforced aluminum matrix composite material powder, and the process steps are as follows:
(1) and (3) filling the mixed aluminum-based composite material powder 1 into a pure aluminum sheath 2, and vibrating or tamping the pure aluminum sheath to ensure that the apparent density of the pure aluminum sheath is 50-70% of the theoretical density. The jacket 2 is made of commercially pure aluminum, the dimensions of which are determined by the billet size.
(2) Covering 1-10 layers of shielding aluminum foils 3 with random holes (each layer of shielding aluminum foil is 0.5-5mm in thickness, the positions of the random holes 3-10 on the shielding aluminum foil are 0.1-0.5mm in diameter) on the upper surface of the composite material powder 1, and welding a covering sleeve 4 with an exhaust pipe.
(3) Several jackets 2 with exhaust pipes are placed in a heating furnace 11. The sheath 2 with the exhaust tube is connected with an air inlet 14 of the decompression chamber through a vacuum hose 12 and a vacuum valve A13.
(4) A digital vacuum gauge 19 is provided on the controllable decompression chamber 15. The controllable decompression chamber 15 is connected with the vacuum unit 18 through the decompression chamber air outlet 16 and the vacuum valve B17.
(5) At normal temperature, the vacuum unit 18 is started with both the vacuum valve a 13 and the vacuum valve B17 closed. The vacuum valve B17 is opened, and the vacuum degree in the controllable decompression chamber 15 is observed by the digital vacuum gauge 19, when reaching 1X 10-2After the proper value between Pa and 9900Pa, the vacuum valve B17 is closed, the vacuum valve A13 is opened to the number of the decompression chamberAfter the reading of the vacuum meter is basically stable, closing the vacuum valve A13 to complete one-time sheath pressure reduction operation; after several times of decompression operation, the vacuum degree in the decompression chamber and the sheath can reach 1-9 x 10- 2Pa, opening a vacuum valve A13 and a vacuum valve B17, starting heating the sheath, heating to the process required temperature, keeping the process required time, and keeping the vacuum degree at 1 x 10-2-9×10-2Pa, in the heating process, the sheath is deflated, the vacuum degree fluctuation occurs, the temperature is kept at the fluctuation temperature point, and the heating is continued after the vacuum fluctuation disappears. And (5) after the heating and heat preservation process is finished, closing the vacuum valve A13 and the vacuum valve B17, sealing the exhaust tube, taking the sheath out of the heating furnace, and finishing the vacuum degassing method process.
Example 1
The aluminum matrix composite material used in the embodiment is a SiC/2024Al composite material, the volume fraction of SiC particles is 15%, the weight of the material is 9kg, and the diameter of the primary blank is 150 mm.
The mixed composite material powder is filled into an industrial pure aluminum sheath with the inner diameter of 150mm and the height of 320mm, and the height of the powder is controlled to ensure that the apparent density is 60 percent. The surface of the composite powder was covered with 4 layers of shielding aluminum foil with a thickness of 0.5mm made of industrial pure aluminum, and 5 holes of 0.5mm were randomly punched. And welding the upper cover of the aluminum sheath with the exhaust tube with the aluminum sheath. And putting a plurality of welded aluminum sheaths into a heating furnace. The aluminum sheath is connected with the air inlet of the controllable decompression chamber through an exhaust pipe, a vacuum valve A and a vacuum hose of the aluminum sheath; a digital vacuum gauge capable of displaying the pressure in the controllable decompression chamber is arranged on the controllable decompression chamber; the air outlet of the controllable decompression chamber is connected with the vacuum unit through a vacuum valve B. And starting the vacuum unit under the condition that the vacuum valve A and the vacuum valve B are both closed at normal temperature. And opening the vacuum valve B, observing the vacuum degree in the controllable decompression chamber through a digital vacuum gauge, closing the vacuum valve B when 8000Pa is reached, opening the vacuum valve A, and closing the vacuum valve A after the numerical vacuum gauge of the decompression chamber is basically stable, thereby completing one sheath decompression operation. After several times of decompression operation, the vacuum degree of each decompression chamber is required to be 7000Pa, 5000Pa, 3000Pa, 1000Pa, 1Pa and 9 multiplied by 10 in sequence-2Pa. The vacuum degree in the decompression chamber and the aluminum sheath reaches 9 multiplied by 10-2After Pa, opening the vacuum valve A and the vacuum valve B, and starting to heat the aluminum sheath. Heating to the required temperature and maintaining the temperature for the required time, wherein the vacuum degree is maintained at not more than 9 × 10-2Pa. In the heating process, air is released in the aluminum sheath, the fluctuation of the vacuum degree occurs, the temperature is preserved at the fluctuation temperature point, and the heating is continued after the vacuum fluctuation disappears. And after the heating and heat preservation process section is finished, closing the vacuum valve A and the vacuum valve B, sealing the exhaust pipe, taking the aluminum sheath out of the heating furnace, and finishing the vacuum degassing method process.
In the original process, the aluminum foil is not shielded in the aluminum sheath, the controllable pressure reduction bin is not arranged in the vacuum pipeline, and the composite powder is directly exposed under vacuum suction. And the shielding aluminum foil and the controllable pressure reduction bin are not arranged, so that the vacuum suction strength is difficult to control in the vacuum degassing process, and the composite material powder is easy to be pumped into a vacuum pipeline from the sheath and even enters the vacuum unit. Through multiple process practice statistics, the powder loss of each ingot in the original process is between 800-1600 g.
In the embodiment, by using the vacuum degassing method with the controllable decompression chamber, compared with the original process, the powder loss of each billet is reduced by at least 50 wt%, the heating and heat-preserving process time of the sheath is shortened by 2-5 hours and is shortened by more than 3% compared with the original process, the production cost of products is effectively reduced, and the production efficiency is improved.

Claims (4)

1.一种颗粒增强铝基复合材料粉末的除气方法,其特征在于,该方法包括如下步骤:1. a degassing method for particle-reinforced aluminum-based composite material powder, characterized in that the method comprises the steps: (1)将混合处理后的颗粒增强铝基复合材料粉末装入包套中,经振动或捣实工艺,使其松装密度至理论密度的50%-70%;(1) Put the mixed-processed particle-reinforced aluminum-based composite powder into the package, and make the bulk density to 50%-70% of the theoretical density through vibration or tamping process; (2)在复合材料粉末上表面覆盖1-10层遮挡铝箔,每层遮挡铝箔厚度在0.5-5mm之间,遮挡铝箔上随机位置打有3-10处直径为0.1-0.5mm的孔洞,然后焊好带有抽气管的包套上盖;(2) Cover the upper surface of the composite powder with 1-10 layers of shielding aluminum foil, the thickness of each layer of shielding aluminum foil is between 0.5-5mm, and there are 3-10 holes with a diameter of 0.1-0.5mm at random positions on the shielding aluminum foil, and then Weld the upper cover of the bag with the exhaust pipe; (3)将装有复合材料粉末的包套放入加热炉内,通过抽气管、真空软管、真空阀A与可控减压舱进气口连接;可控减压舱上有能显示舱内压力的数字真空计;可控减压舱出气口通过真空阀B与真空机组连接;(3) Put the package containing the composite material powder into the heating furnace, and connect it with the air inlet of the controllable decompression chamber through the exhaust pipe, vacuum hose, and vacuum valve A; there is a display chamber on the controllable decompression chamber. Digital vacuum gauge for internal pressure; the air outlet of the controllable decompression chamber is connected to the vacuum unit through the vacuum valve B; (4)启动真空机组,打开真空阀B,观察数字真空计示数,当达到1×10-2Pa-9900Pa后,关闭真空阀B,打开连接包套抽气管的真空阀A,至数字真空计示数基本稳定后,关闭真空阀A,完成一次包套减压操作;(4) Start the vacuum unit, open the vacuum valve B, and observe the digital vacuum gauge. When it reaches 1 × 10 -2 Pa-9900Pa, close the vacuum valve B, open the vacuum valve A connected to the envelope exhaust pipe, and reach the digital vacuum. After the count is basically stable, close the vacuum valve A to complete a decompression operation of the envelope; (5)经数次减压操作,直至减压舱及包套内真空度达到1×10-2-9×10-2Pa,打开真空阀A和真空阀B,开始加热包套;加热过程中,包套内发生放气,出现真空度波动,在波动温度点保温,待真空波动消失后继续加热;(5) After several decompression operations, until the vacuum degree in the decompression chamber and the envelope reaches 1 × 10 -2 -9 × 10 -2 Pa, open the vacuum valve A and the vacuum valve B, and start the heating of the envelope; the heating process During the heating process, outgassing occurs in the envelope, and the vacuum degree fluctuates. The temperature is kept warm at the fluctuating temperature point, and the heating is continued after the vacuum fluctuation disappears; (6)加热及保温过程结束,关闭真空阀A、真空阀B,封死抽气管,将包套从加热炉中取出,完成真空除气过程。(6) After the heating and heat preservation process is over, close the vacuum valve A and the vacuum valve B, seal the exhaust pipe, take out the jacket from the heating furnace, and complete the vacuum degassing process. 2.如权利要求1所述的颗粒增强铝基复合材料粉末的除气方法,其特征在于:所述可控减压舱为不锈钢制耐压壳体,容积大于拟处理包套容积之和的2倍,内表面经打磨抛光。2. The degassing method for particle-reinforced aluminum-based composite material powder according to claim 1, characterized in that: the controllable decompression chamber is a stainless steel pressure-resistant shell, and the volume is greater than the sum of the volume of the package to be processed. 2 times, the inner surface is ground and polished. 3.如权利要求1所述的颗粒增强铝基复合材料粉末的除气方法,其特征在于:所述可控减压舱的出气口的数量与真空机组数量相同,其位置高于进气口;进气口直径在20-60mm之间,数量等于拟处理包套数量。3. The degassing method for particle-reinforced aluminum-based composite material powder according to claim 1, wherein the number of air outlets of the controllable decompression chamber is the same as the number of vacuum units, and its position is higher than the air inlets ; The diameter of the air inlet is between 20-60mm, and the number is equal to the number of packages to be processed. 4.如权利要求1所述的颗粒增强铝基复合材料粉末的除气方法,其特征在于:所述可控减压舱的数字真空计的测量范围为从常压至1×10-5Pa,测量精度为±1%读数。4 . The degassing method for particle-reinforced aluminum matrix composite powder according to claim 1 , wherein the measurement range of the digital vacuum gauge of the controllable decompression chamber is from normal pressure to 1×10 −5 Pa. 5 . , the measurement accuracy is ±1% of reading.
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