CN114045424B - Mixed powder for additive manufacturing and preparation method thereof - Google Patents

Mixed powder for additive manufacturing and preparation method thereof Download PDF

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CN114045424B
CN114045424B CN202111340330.1A CN202111340330A CN114045424B CN 114045424 B CN114045424 B CN 114045424B CN 202111340330 A CN202111340330 A CN 202111340330A CN 114045424 B CN114045424 B CN 114045424B
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powder
frequency
vibration
table body
mixing
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CN114045424A (en
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王理林
王志军
林鑫
黄卫东
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Northwestern Polytechnical University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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Abstract

The invention discloses mixed powder for additive manufacturing and a preparation method thereof. The method is suitable for flexible and simple requirements on powder component regulation in scientific research, and is also suitable for high-efficiency and large-scale requirements in industrial production. The invention can realize the component regulation of the powder without changing the original sphericity and fluidity of the powder. This enables for powder bed additive manufacturing techniques without compromising the powder lay-up quality of the powder, i.e. even spreading and high bulk density of the powder layer; for the synchronous powder feeding and additive manufacturing technology, the powder feeding stability can be maintained, and the powder blocking risk of a powder nozzle is reduced, so that the mixed powder is ensured to meet the requirement of additive manufacturing formability.

Description

Mixed powder for additive manufacturing and preparation method thereof
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to mixed powder for additive manufacturing and a preparation method thereof.
Background
Additive manufacturing is a recently developed advanced numeric manufacturing technology, and has been widely applied in the fields of aerospace, biomedical, automobiles and the like. The powder is one of the most commonly used raw material modes in additive manufacturing technology, such as 15-53 microns for selected area laser melting additive manufacturing technology, 45-105 microns for electron beam selected area laser melting additive manufacturing technology, and 75-200 microns for laser direct energy deposition technology (or laser stereolithography technology). When certain adjustments are made to the alloy composition or another compound is added to the alloy, one way is to re-powder the alloy by melting the alloy, which is a long period, costly, and sometimes not even technically feasible. Another way is by mixing multiple powders for additive manufacturing, which is straightforward and flexible. At present, the powder mixing method has the problems of mechanical mixing, ball milling, chemical plating and the like, such as uneven powder mixing, damage to additive manufacturing formability due to powder deformation, low powder mixing efficiency and the like, and the components of the additive manufacturing formed sample are uneven if the powder to be melted is mixed unevenly due to high additive manufacturing forming speed; powder deformation can reduce powder flowability and bulk density, and can easily cause formation of additive manufacturing forming defects; the powder mixing efficiency is low, and the industrial production cannot be satisfied. Therefore, these powder mixing modes are often difficult to be applied to the technical field of additive manufacturing.
On the other hand, the existing vibration mixer is usually aimed at mixing liquid and organic powder, but for mixing metal powder with high density, only 0.1-0.3kg of metal powder can be mixed at a time, and the efficiency of the vibration mixer has no obvious advantage compared with mechanical mixing or ball milling, and cannot meet the requirement of large-scale application. Due to the strength and fatigue life limitations of the mechanical mechanism designed springs and other parts, the existing vibration mixer cannot improve the efficiency and scale of metal powder mixing by simply amplifying the parts and vibration power.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides mixed powder for additive manufacturing and a preparation method thereof, so as to solve the technical problems that the powder mixing efficiency is low, and the mixed powder is not suitable for the technical field of additive manufacturing due to uneven components of formed samples or forming defects.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
a hybrid powder for additive manufacturing comprising a composite host powder and an additional powder dispersed on the surface of the host powder or a portion of the additional powder infiltrated into the host powder;
the main powder is aluminum alloy, titanium alloy, high-entropy alloy, steel or high-temperature alloy;
the additional powder is metal powder, non-metal simple substance powder, carbide, boride or nitride;
the main powder and the additional powder are compounded by mixing vibration.
The invention further improves that:
preferably, the host powder is in the micrometer scale and the additional powder is in the micrometer or nanometer scale.
A method of preparing a mixed powder for additive manufacturing, comprising the steps of:
step 1, placing main powder and additional powder together in a powder mixing container to form mixed powder, and placing the powder mixing container on a vibrating table body;
step 2, washing the inside of the powder mixing container;
step 3, setting the vibration frequency range of the vibration table body as f min ～f max Setting a first acceleration and a compression factor;
step 4, vibrating the table body from f min Starting to vibrate, increasing the vibration frequency with a set first acceleration until the vibration frequency is increased to f max The method comprises the steps of carrying out a first treatment on the surface of the Observing the vibration degree of the mixed powder in the process, and recording the corresponding frequency when the vibration degree of the mixed powder is the strongest; when the oscillation degree of the mixed powder is most intense, the mixed powder is contacted with the upper cover plate of the mixing and separating container, and the frequency is the optimal frequency f best Or an optimal frequency interval (f 1 ，f 2 )；
Step 5, resetting the vibration frequency range of the vibration table body, if the mixed powder has the optimal frequency f best Setting residence time, vibrating table body to f best Vibrating at frequency, and staying for a set residence time until the vibration is finished; if there is an optimal frequency interval (f 1 ，f 2 ) Setting a second acceleration value and a dwell time, vibrating the table body from f 1 Starting to vibrate, stopping at a second acceleration value for a set residence time, and continuously increasing the vibration frequency until the vibration frequency is increased to f 2 Ending the vibration;
and 6, taking out the mixed powder after the powder mixing is finished for later use.
Preferably, in step 1, the powder mixing container is fixedly connected with the vibrating table body.
Preferably, in the step 1, the mixed powder container is washed by argon for 1-3min at a washing flow rate of 10-30 cm 3 /min。
Preferably, in step 4, if the oscillation of the powder is always gentle, f is reset min And f max 。
Preferably, in step 5, f 1 ＝f best -(5～40)HZ，f 2 ＝f best +(10～40)HZ。
Preferably, in step 5, if f is not found in the powder mixing process best When the powder mixing process is carried out, the table body of the vibration table is changed from f 1 Starting to vibrate, staying for a set residence time, increasing the speed at a second acceleration value, continuously increasing the vibration frequency, and continuously staying for the residence time every time the vibration frequency is increased until the vibration frequency is increased to f 2 Ending the vibration; if f is present best At that time, vibrating for a set time at that frequency;
the powder mixing process is repeated for a plurality of times.
Preferably, a heat dissipation process and a gas washing process are arranged between the two powder mixing processes.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses mixed powder for additive manufacturing, which comprises main powder and additional powder, wherein the main powder and the additional powder are compounded together in a mixing vibration mode, so that various types of powder for additive manufacturing can be prepared by the method, the additional powder is uniformly distributed on the surface of the main body after mixing, certain difference exists in morphology according to the adding amount of the additional powder before mixing, and the more the adding amount is, the more the additional powder is attached on the surface of the main body, and even the whole main body powder particles can be covered; in addition, infiltration of additional powder into the bulk powder can be achieved by this method for certain powders (e.g., soft aluminum alloy powders). The mixed powder prepared by the method is uniformly and efficiently mixed by optimizing to obtain the optimal vibration frequency (the vibration amplitude of the mixed powder can be maximum when the frequency vibrates). The powder after mixing can ensure that the fluidity and the laser metering yield are similar to those of the main powder before mixing, and the quality of the powder is not affected.
The invention discloses a preparation method of mixed powder for additive manufacturing, which realizes efficient and uniform mixing of powder through vibration and ensures the fluidity of the powder at the same time, so as to be used by additive manufacturing technology. The method is suitable for flexible and simple requirements on powder component regulation in scientific research, and is also suitable for high-efficiency and large-scale requirements in industrial production. The gas filling (inert gas) protection is carried out in the whole process before the vibration process, on one hand, the gas filling can reduce the content of gas (such as oxygen) reacting with alloy powder, ensure that the oxygen content of the powder is not increased, take away the moisture in the atmosphere, and improve the powder mixing effect. Therefore, the invention can realize the component regulation of the powder without changing the original sphericity and fluidity of the powder. This enables for powder bed additive manufacturing techniques without compromising the powder lay-up quality of the powder, i.e. even spreading and high bulk density of the powder layer; for the synchronous powder feeding and additive manufacturing technology, the powder feeding stability can be maintained, and the powder blocking risk of a powder nozzle is reduced, so that the mixed powder is ensured to meet the requirement of additive manufacturing formability. In the subsequent additive manufacturing process, the metal powder with high sphericity and uniform mixing is obtained by the mixing method, the fluidity of the powder can be improved in the additive manufacturing process, the laser absorptivity is improved, the powder layer is uniform and flat in the powder spreading process, the powder stacking density can be kept at a high level, the powder feeding stability can be improved, and the powder blocking risk of a powder nozzle is reduced. In the final molded sample, voids and defects can be reduced, and the sample components can be made uniform.
Drawings
FIG. 1 is a block diagram of an apparatus of the present invention;
FIG. 2 is an SEM image (b) surface magnified view of (a) CoCrFeNi-mixed WC of a CoCrFeNi high entropy alloy (particle size 15-53 um) mixed with 1wt% WC nano-powder (particle size 30-50 nm);
FIG. 3 is an overall enlarged view of a CoCrFeNi high entropy alloy (particle size 15-53 um) mixed with 1wt% TiC nanopowder (particle size 40 nm), wherein (a) is a CoCrFeNi high entropy alloy mixed with 1wt% TiC nanopowder powder particles; (b) Is the distribution diagram of TiC nano powder on the surface of the CoCrFeNi high-entropy alloy.
FIG. 4 shows a CoCrFeNi high entropy alloy (particle size 15-53 um) mixed 1wt％Y 2 O 3 Nanopowder (particle size 10-30 nm), wherein (a) is a CoCrFeNi high entropy alloy mixed with 1wt% Y 2 O 3 An overall enlarged view of the nano-powder particles; (b) Is Y 2 O 3 Distribution pattern of nano powder on the surface of CoCrFeNi high-entropy alloy.
FIG. 5 is a mixture of IN625 superalloy powder (particle size 15-53 um) with 1wt% Y 2 O 3 Nanopowder (particle size 10-30 nm), wherein (a) initial IN625 powder, (b) Y 2 O 3 Nanopowder, (c) Y 2 O 3 An enlarged view of the nano powder agglomerate, (d) mixed powder, (e) and (f) powder Y element and O element energy spectrum scan;
FIG. 6 is a graph of macro features of a mixed powder of Ti55531 titanium alloy powders (particle size 45-150 um) and B powders (particle size 100 um), wherein (a) is Ti55531 titanium alloy powder and B powder; (B) is a distribution pattern of the B powder on the Ti55531 titanium alloy surface.
FIG. 7 is a graph of AlSi10Mg alloy powder (particle size 50-150 um) mixed with 1wt% TiB 2 Nanopowder (average particle size 500 nm), wherein (a) is AlSi10Mg alloy powder mixed with 1wt% TiB 2 An overall enlarged view of the nano-powder particles; (b) Is TiB 2 Distribution of nanopowder on AlSi10Mg surface.
Wherein, 1-cooling fan; 2-vibrating table body; 3-a powder mixing container; 4-a first sensor; 5-power supply; 6-argon source; 7-an upper computer; 8-quick plug; 9-cover plate; 10-a bottom plate; 11-a second sensor.
Detailed Description
The invention is described in further detail below with reference to the attached drawing figures:
in the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., are based on directions or positional relationships shown in the drawings, are merely for convenience of description and simplification of description, and do not indicate or imply that the apparatus or element to be referred to must have a specific direction, be constructed and operated in the specific direction, and thus should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixed or removable, for example; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The invention discloses a mixing device and a mixing method for additive manufacturing, referring to fig. 1, the mixing device comprises a vibrating table body 2, a powder mixing container 3 is arranged on the vibrating table body 2, and the powder mixing container 3 is detachably connected with the vibrating table body 2.
Specifically, the vibrating table body 2 is fixedly provided with a bottom plate 10, the bottom plate 10 is detachably connected with the powder mixing container 3, the upper end of the powder mixing container 3 is provided with a cover plate 9, and the cover plate 9 and the bottom plate 10 are all made of aluminum alloy plates. The cover plate 9 and the bottom plate 10 are connected by 8 bolts. Two quick plugs are arranged on the cover plate 9 and are used for being connected with the argon source 6.
The base plate 10 is provided with a first sensor 4, the vibrating table body 2 is provided with a second sensor 11, the first sensor 4 and the second sensor 11 are connected with the upper computer 7, and the upper computer 7 monitors the vibration frequency of the powder mixing container 3 through the vibration frequency acquired by the first sensor 4 and the second sensor 11; the upper computer 7 controls the acceleration of the vibration table body 2 at the same time, and the upper computer 7 controls the vibration frequency and the acceleration of the vibration table body 2 through a vibration controller.
The power supply 5 is connected with the vibrating table body 2 and the cooling fan 1 at the same time, so that power is supplied to two devices at the same time, the cooling fan 1 is connected with the vibrating table body 1, and the cooling fan 1 is used for cooling heat generated by current heating and motor movement in the vibrating table body 2.
The principle of the industrial-level vibrating table of the invention is that large thrust is provided by electromagnetic control, and the vibration parameter selection range is very wide, for example, the exciting force can be from small 1960N (moving coil weight 2 Kg) to large 156800N (moving coil weight 160 Kg). Under the acceleration of 60G (G is gravity acceleration), the weight of the small vibration table is 1960/(60×9.8) -2=1.3 Kg each time, and the weight of the small vibration table is 156800/(60×9.8) -160=107 Kg each time. Therefore, by adopting the electromagnetic control vibrating table and combining the device designed by the invention, powder can be mixed in a high-efficiency and large-scale manner.
The process of mixing powder by the device comprises the following steps:
1. placing the powder of the powder to be mixed in the powder mixing container 3, placing the powder mixing container 3 on the vibrating table body 2, fixing the powder mixing container 3 on the vibrating table body 2, more specifically, aligning the screw holes of the bottom plate 10 with the screw holes above the vibrating table body 2, covering the cover plate 9, enabling 8 bolts to pass through the coaxial screw holes of the cover plate 9 and the bottom plate 10, screwing in the screw holes of the vibrating table body 2, screwing in the screws, and completely fixing the cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. 2 quick plugs 8 are all opened, a switch is opened at an argon decompression valve, the flow rate of argon is regulated, and the flow rate is 10-30 cm 3 And (3) during/min, the argon pipeline is connected into 1 quick plug 8, the interior of the powder mixing container 8 is scrubbed for 1-3min, the argon pipeline is pulled out, and the 2 quick plugs 8 are closed in time.
3. A first sensor 4 is fixed to the lower cover plate of the powder mixing container 3 for monitoring the vibration frequency during the powder mixing process. A second sensor 11 is fixed on the vibrating table body 2 for monitoring and controlling parameters in the powder mixing process. The vibration frequency of two devices is monitored simultaneously to two sensors, prevents that vibration frequency of shaking table stage body 2 can't abundant transmission to mix in the powder container 3, influences the powder effect.
4. The upper computer 7 sets the vibration frequency range of the vibration table body 1 as f min -f max Setting a first acceleration and a compression factor, and starting powder mixing;
5. determining an optimal vibration frequency, starting from f, the vibration frequency of the vibrating table body 1 min Starting to vibrate, and starting to increase the vibration frequency with the set acceleration value until the vibration frequency is increased to f max Observing the vibration degree of the powder, and recording the corresponding frequency when the vibration degree of the powder is most intenseThe frequency is the optimal frequency value f best . In the vibration process, if the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. In the powder mixing process, the vibration range f is set again through the upper computer 1 -f 2 Or f best ，f min ＜f 1 ＜f best ，f best ＜f 2 ＜f max Dwell time and second acceleration value such that the vibrating table body is at f 1 And f 2 Vibrating in between; the vibration frequency of the vibrating table body 1 is from f 1 Starting vibration, continuously accelerating with a second acceleration value during vibration, and then continuously rising to f max Ending the vibration; or at f best The frequency vibrates for a certain period of time.
7. After powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing.
The mixed powder prepared by the above preparation method comprises composite main powder and additional powder, wherein the additional powder is dispersed on the surface of the main powder or part of the additional powder is permeated into the main powder; the main powder is aluminum alloy, titanium alloy, high-entropy alloy, steel or high-temperature alloy; the additional powder is metal powder, carbide, boride or nitride; the host powder is micron-sized and the additional powder is micron-sized or nano-sized.
The following is a further description of specific embodiments:
example 1
1. And (2) mounting: firstly, pouring WC with a certain mass into a powder mixing container 3, then pouring CoCrFeNi high-entropy alloy powder with a weight of about 1Kg into the powder mixing container 3, covering the WC powder, preventing WC from being blown away, placing the powder mixing container 3 above a vibrating table body 2, requiring that screw holes of a bottom plate 10 are aligned with screw holes above the vibrating table body 2, covering an Al alloy cover plate 9, enabling 8 bolts to pass through the screw holes of the 2 Al alloy cover plates 9, screwing the 8 bolts into the screw holes of the vibrating table body 2, screwing screws, and completely fixing the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. Opening a switch at an argon decompression valve of an argon source 6, adjusting the flow of the argon until the flow rate is 10-30 cm 3 And at the time of/min, an argon pipeline is connected into the quick plug 8 for gas washing. After 3 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 40 and 200Hz respectively min 40 and f max The accelerations were defined as 35g at 200Hz. In the default sweep frequency 1 column, the start point frequency is defined as 40Hz and the end point frequency is defined as 200Hz. The frequencies 40 and 200Hz are input at the start and end points of the default compression factor 1 column, respectively, with the compression factor defaulting to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. This frequency is the optimum frequency value, in this embodiment 100Hz. If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: the basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column, and the start frequency is defined as 100Hz, i.e. the optimal frequency value. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing. As shown in figure 2, the mixed powder has uniform distribution of WC powder on the surface of the powder, and white WC powder is relatively fine, but the agglomeration phenomenon is not found, and the WC powder has uniform distribution on the surface of the CoCrFeNi high-entropy alloy powder, so that the powder can be used for additive manufacturing.
Example 2
1. And (2) mounting: firstly pouring TiC with a certain mass into a powder mixing container 3, then pouring about 1Kg of CoCrFeNi high-entropy alloy powder into the powder mixing container 3, covering the TiC powder to prevent TiC from being blown away, placing the powder mixing container 3 above a vibrating table body 2, requiring that screw holes of a bottom plate 10 are aligned with screw holes above the vibrating table body 2, covering an Al alloy cover plate 9, enabling 8 bolts to pass through the screw holes of 2 Al alloy cover plates 9, screwing in the screw holes of the vibrating table body 2, screwing in screws, and completely fixing the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. And opening a switch at an argon decompression valve of the argon source 6, adjusting the flow of the argon, and when the flow rate is 10-30 cm < 3 >/min, connecting an argon pipeline into the quick plug 8 for gas washing. After 1 minute of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 40 and 200Hz respectively min 40 and f max The accelerations were defined as 35g at 200Hz. In the default sweep frequency 1 column, the start point frequency is defined as 40Hz and the end point frequency is defined as 200Hz. At the start point of the default compression factor 1 columnThe end point is entered at frequencies 40 and 200Hz, respectively, with a compression factor defaulting to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. This frequency is the optimum frequency value, in this example 90Hz. If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: the basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column, and the start frequency is defined as 90Hz, i.e. the optimal frequency value. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing. The mixed powder is shown in fig. 3, the granular white TiB powder is uniformly distributed on the surface of the CoCrFeNi high-entropy alloy powder, the TiB powder is not agglomerated, and the powder can be used for additive manufacturing due to good dispersibility.
Example 3
1. And (2) mounting: first, Y of a certain mass 2 O 3 Pouring into the powder mixing container 3, pouring about 1Kg of CoCrFeNi high entropy alloy powder into the powder mixing container 3, and covering Y 2 O 3 Powder, preventing Y2O3 from being blown away, placing the powder mixing container 3 above the vibrating table body 2, requiring aligning screw holes of the bottom plate 10 with nut holes above the vibrating table body 2, covering the Al alloy cover plate 9, passing 8 bolts through the screw holes of the 2 Al alloy cover plates 9, screwing in the nuts of the vibrating table body 2, screwing in the screws,the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 are completely fixed together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. And opening a switch at an argon decompression valve of the argon source 6, adjusting the flow of the argon, and when the flow rate is 10-30 cm < 3 >/min, connecting an argon pipeline into the quick plug 8 for gas washing. After 2 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 40 and 200Hz respectively min 40 and f max The accelerations were defined as 35g at 200Hz. In the default sweep frequency 1 column, the start point frequency is defined as 40Hz and the end point frequency is defined as 200Hz. The frequencies 40 and 200Hz are input at the start and end points of the default compression factor 1 column, respectively, with the compression factor defaulting to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. This frequency is the optimum frequency value, in this example 70Hz. If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: the basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column, and the start frequency is defined as 70Hz, i.e. the optimal frequency value. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing. The mixed powder is shown in FIG. 4, fine Y 2 O 3 The powder is uniformly distributed on the surface of the powder, and Y is added in a small amount 2 O 3 The powder does not completely cover the surface of the CoCrFeNi high entropy alloy powder, but its distribution is very uniform.
Example 4
1. And (2) mounting: first, Y of a certain mass 2 O 3 Pouring into the powder mixing container 3, pouring about 1Kg of IN625 superalloy powder into the powder mixing container 3, covering oxide powder, and preventing Y 2 O 3 The metal powder is blown away, the powder mixing container 3 is placed above the vibrating table body 2, the screw holes of the bottom plate 10 are required to be aligned with the nut holes above the vibrating table body 2, the Al alloy cover plate 9 is covered, 8 bolts penetrate through the screw holes of the 2 Al alloy cover plates 9 and are screwed into the nuts of the vibrating table body 2, the screws are tightened, and the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 are completely fixed together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. Opening a switch at an argon decompression valve of an argon source 6, adjusting the flow of the argon until the flow rate is 10-30 cm 3 And at the time of/min, an argon pipeline is connected into the quick plug 8 for gas washing. After 3 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 40 and 200Hz respectively min 40 and f max The accelerations were defined as 35g at 200Hz. In the default sweep frequency 1 column, the start point frequency is defined as 40Hz and the end point frequency is defined as 200Hz. At defaultThe start and end points of the compression factor 1 column are input at frequencies 40 and 200Hz, respectively, and the compression factor defaults to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. This frequency is the optimum frequency value, in this example 88Hz. If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: the basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column, and the start frequency is defined as 80Hz, i.e. the optimal frequency value. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing. The mixed powder is shown in FIG. 5, Y 2 O 3 The powder is uniformly distributed on the surface of the powder and Y 2 O 3 The powder almost completely covers the whole IN625 superalloy powder, forming a thin layer of Y on the IN625 superalloy powder surface 2 O 3 Powder layer, which realizes Y 2 O 3 The uniform mixing of the powders can be used for additive manufacturing.
Example 5
1. And (2) mounting: firstly pouring a certain mass of B into a powder mixing container 3, then pouring about 1Kg of Ti55531 titanium alloy powder into the powder mixing container 3 to cover the B powder and prevent the B powder from being blown away, placing the powder mixing container 3 above a vibrating table body 2, requiring that screw holes of a bottom plate 10 are aligned with screw holes above the vibrating table body 2, covering an Al alloy cover plate 9, enabling 8 bolts to pass through the screw holes of the 2 Al alloy cover plates 9, screwing the 8 bolts into the screw holes of the vibrating table body 2, screwing screws, and completely fixing the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. Opening a switch at an argon decompression valve of an argon source 6, adjusting the flow of the argon until the flow rate is 10-30 cm 3 And at the time of/min, an argon pipeline is connected into the quick plug 8 for gas washing. After about 1-3 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 15 and 100Hz respectively min Is 15 and f max Acceleration was defined as 15g for 100Hz. In the default sweep frequency 1 column, the start point frequency is defined as 15Hz and the end point frequency is defined as 100Hz. The frequencies 15 and 100Hz are input at the start and end points of the default compression factor 1 column, respectively, and the compression factor defaults to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. The frequency is an optimal frequency value, and in this embodiment, there is no optimal frequency, and there is an optimal frequency interval (20-30 Hz). If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: according to the basic setting of step 1, 20Hz and 30Hz, i.e. f, are selected 1 20Hz, f 2 30Hz; as a start point frequency and an end point frequency, respectively. The basic setup of step 1 is repeated. Adding "resident" type in the Programming Table 1 column,. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing. As shown in fig. 6 (B), the mixed powder is shown in fig. 6, the micron-sized B powder is attached to the surface of the Ti55531 titanium alloy powder, and the smaller B powder becomes the planetary powder of the larger Ti55531 titanium alloy powder, and as can be observed from the overall effect diagram (a), the B powder is uniformly distributed on the surface of the Ti55531 titanium alloy powder, and can be used for additive manufacturing.
Example 6
1. And (2) mounting: firstly, 1Kg of AlSi10Mg alloy powder is poured into the powder mixing container 3, and then a certain mass of TiB is poured into the powder mixing container 2 Pouring the mixture into the powder mixing container 3, placing the powder mixing container 3 above the vibrating table body 2, requiring aligning screw holes of the bottom plate 10 with nut holes above the vibrating table body 2, covering the Al alloy cover plate 9, enabling 8 bolts to pass through the screw holes of the 2 Al alloy cover plates 9, screwing in the nuts of the vibrating table body 2, screwing in the screws, and completely fixing the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. And opening a switch at an argon decompression valve of the argon source 6, adjusting the flow of the argon, and when the flow rate is 10-30 cm < 3 >/min, connecting an argon pipeline into the quick plug 8 for gas washing. After about 3 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. In the sweep spectrum 1The frequencies are added in a column with two rows of frequencies of 0 and 50Hz, respectively, i.e. f min Is 0 and f max The accelerations were defined as 35g at 50Hz. In the default sweep frequency 1 column, the start point frequency is defined as 0Hz and the end point frequency is defined as 50Hz. The frequencies 0 and 50Hz are respectively input at the starting point and the ending point of the default compression factor 1 column, and the compression factor defaults to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. The frequency is an optimal frequency value, and in this embodiment, there is no optimal frequency, and there is an optimal frequency interval (10-25 Hz). If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: according to the basic setting of step 1, 10Hz and 25Hz, i.e. f, are selected 1 Is 10Hz, f 2 25Hz; as a start point frequency and an end point frequency, respectively. The basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing. The mixed powder is shown in FIG. 7, which shows a nano-scale white TiB 2 The powder is uniformly distributed on the surface of AlSi10Mg alloy powder and TiB is prepared 2 The powder does not have agglomeration phenomenon, has good dispersibility on the surface of AlSi10Mg alloy powder, and can be used for additive manufacturing.
Example 7
1. And (2) mounting: first 1Kg of 316L stainless steelPouring steel alloy powder into the powder mixing container 3, and then pouring a certain mass of Ti 3 N 4 Pouring the mixture into the powder mixing container 3, placing the powder mixing container 3 above the vibrating table body 2, requiring aligning screw holes of the bottom plate 10 with nut holes above the vibrating table body 2, covering the Al alloy cover plate 9, enabling 8 bolts to pass through the screw holes of the 2 Al alloy cover plates 9, screwing in the nuts of the vibrating table body 2, screwing in the screws, and completely fixing the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. And opening a switch at an argon decompression valve of the argon source 6, adjusting the flow of the argon, and when the flow rate is 10-30 cm < 3 >/min, connecting an argon pipeline into the quick plug 8 for gas washing. After about 3 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 0 and 40Hz respectively min Is 0 and f max Acceleration was defined as 35g at 40Hz. In the default sweep frequency 1 column, the start point frequency is defined as 0Hz and the end point frequency is defined as 40Hz. The frequencies 0 and 40Hz are input at the start and end points of the default compression factor 1 column, respectively, and the compression factor defaults to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. This frequency is the optimum frequency value, in this example 9Hz. If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: the basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column, and the start frequency is defined as 9Hz, i.e. the optimal frequency value. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing.
Example 7
1. And (2) mounting: firstly pouring metal Mo powder with a certain mass into a powder mixing container 3, then pouring about 1Kg of pure Ti powder into the powder mixing container 3, covering the metal Mo powder, preventing the metal Mo from being blown away, placing the powder mixing container 3 above a vibrating table body 2, requiring that screw holes of a bottom plate 10 are aligned with screw holes above the vibrating table body 2, covering an Al alloy cover plate 9, enabling 8 bolts to pass through the screw holes of the 2 Al alloy cover plates 9, screwing the 8 bolts into the screw holes of the vibrating table body 2, screwing screws, and completely fixing the upper cover plate 9, the powder mixing container 3 and the vibrating table body 2 together.
2. And (3) gas washing: the 2 quick plugs 8 are all opened. Opening a switch at an argon decompression valve of an argon source 6, adjusting the flow of the argon until the flow rate is 10-30 cm 3 And at the time of/min, an argon pipeline is connected into the quick plug 8 for gas washing. After about 1-3 minutes of purging, the argon line was pulled out and the 2 quick plugs were closed in time.
3. Paste sensor: the first sensor 4 is attached to the floor 10 of the mixing container 3 for monitoring parameters during mixing. A second sensor is stuck to the vibrating table body 2 and is used for controlling parameters in the powder mixing process.
4. The basic arrangement is as follows: opening the operating software clicks on the programming test scheme. Adding two rows of frequencies in a column of the frequency of the sweep spectrum 1, namely f, at 15 and 80Hz respectively min Is 15 and f max The accelerations were defined as 15g at 80Hz. At default scan frequency of 1 column, start pointThe frequency was defined as 15Hz and the end point frequency was defined as 80Hz. The frequencies 15 and 80Hz are input at the start and end points of the default compression factor 1 column, respectively, with the compression factor defaulting to 5. After the setting is completed, a start button is clicked, and the powder mixing process is started.
5. Searching optimal parameters: the naked eye pays attention to the vibration condition of the powder in the powder mixing container, and when the vibration degree of the powder is the most intense (the vibrated powder contacts the upper cover plate), the corresponding frequency at the moment is recorded. This frequency is the optimum frequency value, in this example 25Hz. If the powder oscillation condition is found to be gentle, the starting point frequency, the ending point frequency and the acceleration value can be considered to be adjusted, and the selection of the optimal frequency value is carried out again.
6. Powder mixing process: the basic setup of step 1 is repeated. The "resident" type is added in the schedule table 1 column, and the start frequency is defined as 15Hz, i.e. the optimal frequency value. The residence time was set at 3min in the time series. And then clicks the start button. After 3min, the powder mixing process is finished for 1 time, and the powder is kept for 1min to dissipate heat of the container. The powder mixing process was then repeated 3 times for a total of 12 minutes. And (5) finishing the powder mixing process. It is considered that the air-washing process is performed again after mixing the powder 2 times to ensure the internal atmosphere of the powder mixing container.
7. And (3) disassembly: after powder mixing is finished, the two sensors are firstly taken down, then the bolts are unscrewed, the upper cover plate is taken down, the mixed powder is dried and then poured into other storage devices for sealing and storage, and the powder is used for subsequent additive manufacturing.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (3)

1. A method of preparing a mixed powder for additive manufacturing, comprising the steps of:
step 1, placing main powder and additional powder together in a powder mixing container (3) to form mixed powder, and placing the powder mixing container (3) on a vibrating table body (2);
the main powder is aluminum alloy, titanium alloy, high-entropy alloy, steel or high-temperature alloy;
the additional powder is metal powder, non-metal simple substance powder, carbide, boride or nitride;
the main powder and the additional powder are compounded through mixing vibration; the additional powder is dispersed on the surface of the main powder, or a part of the additional powder is permeated into the main powder;
the main powder is in a micron level, and the additional powder is in a micron level or a nanometer level;
step 2, washing the inside of the powder mixing container (3);
step 3, setting the vibration frequency range of the vibration table body (2) as f min ~f max Setting a first acceleration value and a compression factor; the vibrating table body (2) is from f under the first acceleration min Starting to vibrate, and gradually increasing the vibration frequency to f max The method comprises the steps of carrying out a first treatment on the surface of the Observing the vibration degree of the mixed powder in the process, and recording a corresponding frequency fixed value or a frequency interval when the vibration degree of the mixed powder is the strongest; the frequency of the mixed powder when the oscillation degree is most intense is the optimal frequency f best Or an optimal frequency interval (f 1 ，f 2 ) The method comprises the steps of carrying out a first treatment on the surface of the If the oscillation of the powder is always gentle, f is reset min And f max Repeating the above process until finding the optimal frequency f best Or an optimal frequency interval (f 1 ，f 2 ）；
Step 4, resetting the second acceleration value and the vibration residence time of the vibration table body (2), if the mixed powder has the optimal frequency f best Setting residence time, vibrating table body (2) at f best Vibrating at the frequency until the set residence time is reached, and ending the vibration; if there is an optimal frequency interval (f 1 ，f 2 ) Under the second acceleration, the vibrating table body (2) vibrates from f 1 Starting to vibrate, gradually increasing the vibration frequency to f according to the set residence time 2 Ending the vibration;
f 1 =f best -（5~40）Hz，f 2 =f best +（10~40）Hz；
the powder mixing process is repeated for a plurality of times; a heat dissipation process and a gas washing process are arranged between the two powder mixing processes;
and 5, taking out the mixed powder after the powder mixing is finished for later use.
2. The method of mixing additive manufacturing powder according to claim 1, wherein in step 1, the powder mixing container (3) and the vibrating table body (2) are fixedly connected.
3. The method of mixing additive manufacturing powder according to claim 1, wherein in step 2, the powder mixing container (3) is purged with argon for 1-3min at a purge flow rate of 10-30 cm 3 /min。
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