CN110273120B - Method and device for rapidly nanocrystallizing alloy surface - Google Patents
Method and device for rapidly nanocrystallizing alloy surface Download PDFInfo
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- CN110273120B CN110273120B CN201910697212.2A CN201910697212A CN110273120B CN 110273120 B CN110273120 B CN 110273120B CN 201910697212 A CN201910697212 A CN 201910697212A CN 110273120 B CN110273120 B CN 110273120B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
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- C21D10/00—Modifying the physical properties by methods other than heat treatment or deformation
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D7/00—Modifying the physical properties of iron or steel by deformation
- C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
- C21D7/04—Modifying the physical properties of iron or steel by deformation by cold working of the surface
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Abstract
The invention particularly relates to a method and a device for rapidly nanocrystallizing an alloy surface, which belong to the technical field of alloy nanocrystallization preparation, and aim to solve the technical problem of providing a method and a device for rapidly nanocrystallizing a structure of the surface of an alloy block part, wherein the method and the device adopt the following technical scheme: the method comprises the following steps: 1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover; 2) Shot blasting and hydrogenation-disproportionation treatment: carrying out shot blasting treatment on the sample under the mixed pressure of hydrogen and argon of 1-6 MPa and the temperature of 445-455 ℃; 3) Shot blasting and dehydrogenation-recombination treatment: the sample was subjected to a pressure of 2.0X10 ‑4 ～7.0×10 ‑4 Performing shot blasting treatment under the Pa vacuum degree and the temperature of 445-455 ℃; the invention combines the shot blasting technology and the hydrogenation dehydrogenation technology, reduces the hydrogen pressure and improves the thickness of the nanocrystalline layer on the surface of the block part.
Description
Technical Field
The invention belongs to the technical field of alloy nanocrystallization preparation, and particularly relates to a method and a device for rapidly nanocrystallizing an alloy surface.
Background
In order to expand the application range of the alloy, a method of refining grains is generally adopted to improve the comprehensive performance of the alloy, and at present, high-energy ball milling, equal-channel extrusion, melt rapid quenching and other methods are generally adopted, wherein the methods can only refine the alloy to a micron level, and the grain layer is thinner, has the thickness of about 20 mu m, and can not meet the application requirements of products, so that the application of the alloy is still greatly limited. The hydrogenation dehydrogenation method, namely the HDDR method, is also a common method for nano-alloying an alloy, generally, the alloy powder is subjected to HDDR treatment to nano-alloy powder, and then the nano-alloy powder is sintered, so that the method is complex in operation, needs hydrogen pressure of between 350 and 450 ℃ and between 6 and 7MPa for the application of the block-shaped parts, is inflammable and explosive, and has potential safety hazards.
Disclosure of Invention
The invention overcomes the defects existing in the prior art, provides a method and a device for rapidly nanocrystallizing the structure of the surface of an alloy block part, and reduces H 2 The use amount of the alloy reduces the potential safety hazard, effectively improves the thickness of the nano layer, effectively nanocrystallizes the grain size, and improves the specific stiffness, specific strength and corrosion resistance of the alloy.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot peening and hydro-disproportionation (HD) processing: distributing hydrogen and argon to a reaction bin according to the flow rate ratio of 1:3-1:6, and performing shot blasting, hydrogenation and disproportionation treatment on an alloy block sample under the conditions that the pressure of the reaction bin is 1-6 MPa and the temperature is 445-455 ℃;
3) Shot peening and dehydrogenation-recombination (DR) treatment: the pressure in the reaction chamber was 2.0X10 -4 ～7.0×10 -4 And (3) under the Pa vacuum degree and at the temperature of 445-455 ℃, carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: shut down lowVacuum valve, open high vacuum valve, pump reaction chamber pressure to 2.0X10 -4 ～7.0×10 -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:3-1:6, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches the working pressure of 1-6 MPa;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 8-12 mins, then continuously raising the temperature to 345-355 ℃ for 8-12 mins, and finally continuously raising the temperature to 445-455 ℃ for 2-4 mins;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: shot blasting is carried out on the sample under the conditions of the reaction bin pressure of 1-6 MPa and the temperature of 445-455 ℃ for 0.5-12 h;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 2.0X10 -4 ～7.0×10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 8-12 mins, then continuously raising the temperature to 345-355 ℃ for 8-12 mins, and finally continuously raising the temperature to 445-455 ℃ for 2-4 mins;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 0.5-6 h, a high vacuum valve is in an open state in the process, the reaction bin is continuously vacuumized, and the pressure of the reaction bin is kept to be 2.0 multiplied by 10 -4 ～7.0×10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample;
the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The flow rate of the argon source is 10-50 KPa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 30-60 min.
The heating pipe is a microwave heating pipe.
An apparatus for rapid nanocrystallization of an alloy surface, comprising: the sample is fixed on a sample table of the shot blasting machine, a shot outlet of the shot blasting machine faces the sample, the shot outlet is fixed with the inner wall of a reaction bin of the shot blasting machine, the exhaust pipe is arranged at the upper end of the reaction bin and is used for exhausting gas in the reaction bin, a hydrogen inlet and an argon inlet are arranged on one side wall of the reaction bin, the air inlet end of the hydrogen inlet is communicated with a hydrogen source outside the reaction bin, the air inlet end of the argon inlet is communicated with an argon source outside the reaction bin, one end of the vacuum tube is communicated with the reaction bin, the other end of the vacuum tube is communicated with vacuumizing equipment, the heating tube is further fixed on the inner wall of the reaction bin and is used for heating the reaction bin, the cooling water pipe is further fixed with a snakelike cooling water pipe on the inner wall of the reaction bin and is used for cooling gas in the reaction bin, and a pressure gauge and a thermometer are further fixed in the reaction bin.
The device for rapidly nanocrystallizing the alloy surface further comprises: the nitrogen gas intake pipe, the nitrogen gas intake pipe runs through the storehouse wall of reaction storehouse, the exit end of nitrogen gas intake pipe set up in sample platform below, the exit end of nitrogen gas intake pipe with the reaction storehouse inner wall is fixed, the other end and the liquid nitrogen source intercommunication of nitrogen gas intake pipe.
The vacuum tube includes: one end of the low vacuum tube is communicated with the reaction bin, the other end of the low vacuum tube is communicated with the Roots rotary-vane vacuum pump, one end of the high vacuum tube is communicated with the reaction bin, the other end of the high vacuum tube is communicated with the diffusion pump, and the low vacuum tube and the high vacuum tube are respectively provided with a low vacuum valve and a high vacuum valve.
The shot-blasting machine includes: the device comprises a bin cover, a window, a chip outlet and a motor, wherein the bin cover is used for taking and placing samples, the window is fixed on one side wall of the shot blasting machine, the window is used for observing conditions in a reaction bin, the chip outlet is arranged below the reaction bin and used for discharging chips generated in a reaction treatment process, the motor is fixed at the upper end of the shot blasting machine, an output shaft of the motor is connected with the bottom of a sample table, and the motor is used for driving the sample table to rotate.
Compared with the prior art, the invention has the following beneficial effects.
1. The invention combines the shot blasting technology and the hydrogenation dehydrogenation technology, effectively reduces the higher hydrogen pressure required by HDDR, reduces the hydrogen consumption, reduces the potential safety hazard, improves the thickness of the nanocrystalline layer on the surface of the block part, has the thickness of 40-60 mu m and the grain size of 10-30 nm, and effectively improves the specific stiffness, specific strength and corrosion resistance of the alloy.
2. The invention designs a heating pipe, in the reaction process, the temperature of the reaction bin is firstly increased to 145-155 ℃ for 8-12 mins, then the temperature is continuously increased to 345-355 ℃ for 8-12 mins, finally the temperature is continuously increased to 445-455 ℃ for 2-4 mins, and the reaction bin is heated from slow to fast, so that the formation of a nano layer on the surface of a sample is facilitated.
3. The invention is provided with a rapid cooling system, a cooling water pipe is opened to cool the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample, so that the formed nano layer is favorable to maintain the existing state, and the damage of the nano layer structure caused by slow cooling is prevented.
4. The invention utilizes the mechanical energy of shot blasting bombardment and the high-speed collision friction energy of steel shots and alloy to provide the activation energy of the alloy matrix and hydrogen reaction required by the HDDR process, accelerates the migration and diffusion of hydrogen, accelerates the reaction process, can rapidly nanocrystallize the surface structure of the alloy block part, and improves the working efficiency.
5. The invention utilizes the hydrogen cracking refinement of the alloy and cavitation effect of high-concentration supersaturated dissolved hydrogen by using the HDDR process to improve the efficiency of shot blasting refinement.
6. The invention utilizes the temperature rise of high-speed collision friction of shot blasting and alloy, effectively reduces the temperature required by HDDR, reduces consumption and saves energy.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of a rapid nanocrystallization device for an alloy surface according to the present invention.
FIG. 2 is a schematic diagram of the internal structure of the rapid nanocrystallization device for alloy surfaces according to the invention.
In the figure: 1 is a hydrogen inlet, 2 is an argon inlet, 3 is a shot blasting machine, 4 is an exhaust pipe, 5 is a low vacuum valve, 6 is a high vacuum valve, 7 is a window, 8 is a bin cover, 9 is a nitrogen inlet pipe, 10 is a heating pipe, 11 is a cooling water pipe, 12 is a sample, 13 is a sample stage, 14 is a shot outlet, and 15 is a reaction bin.
Detailed Description
The invention is further illustrated below with reference to specific examples.
Example 1
A method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:3, and performing shot blasting and hydrogenation-disproportionation treatment on the alloy block sample under the conditions that the pressure of the reaction bin is 1MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 2.0X10 -4 Shot blasting and stripping are carried out on the alloy block sample under the Pa vacuum degree and the temperature of 445-455 DEG CAnd (5) carrying out hydrogen-recombination treatment to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 2.0X10 -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:3, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches the working pressure of 1 MPa;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 8mins, then continuously raising the temperature to 345-355 ℃ for 8mins, and finally continuously raising the temperature to 445-455 ℃ for 2mins;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: carrying out shot blasting treatment on the sample for 0.5h under the conditions that the pressure of a reaction bin is 1MPa and the temperature is 445-455 ℃;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmosphere, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by using a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 2.0X10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 8mins, then continuously raising the temperature to 345-355 ℃ for 8mins, and finally continuously raising the temperature to 445-455 ℃ for 2mins;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 0.5h, a high vacuum valve is in an open state in the process, the reaction bin is continuously vacuumized, and the pressure of the reaction bin is kept to be 2.0 multiplied by 10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmosphere, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample; the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 30mins.
The heating pipe is a microwave heating pipe.
An apparatus for rapid nanocrystallization of an alloy surface, comprising: the device comprises a hydrogen inlet 1, an argon inlet 2, a shot blasting machine 3, an exhaust pipe 4, a vacuum pipe, a heating pipe 10 and a cooling water pipe 11, wherein a sample 12 is fixed on a sample table 13 of the shot blasting machine 3, a shot outlet 14 of the shot blasting machine 3 faces to the sample 12, the shot outlet 14 is fixed with the inner wall of a reaction bin 15 of the shot blasting machine 3, the upper end of the reaction bin 15 is provided with the exhaust pipe 4, the exhaust pipe 4 is used for discharging gas in the reaction bin 15, one side wall of the reaction bin 15 is provided with the hydrogen inlet 1 and the argon inlet 2, the air inlet end of the hydrogen inlet 1 is communicated with a hydrogen source outside the reaction bin 15, the air inlet end of the argon inlet 2 is communicated with an argon source outside the reaction bin 15, one end of the vacuum pipe is communicated with the reaction bin 15, the other end of the vacuum pipe is communicated with vacuumizing equipment, the heating pipe 10 is further fixed on the inner wall of the reaction bin 15, the cooling water pipe 11 is further fixed in the reaction bin 15, and the cooling water pipe 11 is further fixed in the reaction bin 15.
The device for rapidly nanocrystallizing the alloy surface further comprises: the nitrogen gas intake pipe 9, nitrogen gas intake pipe 9 runs through the storehouse wall of reaction storehouse 15, the exit end of nitrogen gas intake pipe 9 set up in sample platform 13 below, the exit end of nitrogen gas intake pipe 9 with reaction storehouse 15 inner wall is fixed, the other end and the liquid nitrogen source intercommunication of nitrogen gas intake pipe 9.
The vacuum tube includes: the reaction chamber 15 is communicated with one end of the low vacuum pipe, the Roots rotary-vane vacuum pump is communicated with the other end of the low vacuum pipe, the reaction chamber 15 is communicated with one end of the high vacuum pipe, the diffusion pump is communicated with the other end of the high vacuum pipe, and the low vacuum valve 5 and the high vacuum valve 6 are respectively arranged on the low vacuum pipe and the high vacuum pipe.
The shot-blasting machine 3 includes: the bin cover 8, the window 7, the piece export and the motor, the bin cover 8 is used for getting the sample of putting, the window 7 is fixed in on the lateral wall of shot-blasting machine 3, the window 7 is used for observing the condition in the reaction storehouse 15, the below of reaction storehouse 15 is provided with the piece export, the piece export is used for discharging the piece that produces in the reaction treatment process, the motor is fixed in the upper end of shot-blasting machine 3, the output shaft and the sample platform 13 bottom of motor are connected, the motor is used for driving sample platform 13 rotation.
Example 2
A method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:6, and performing shot blasting and hydrogenation-disproportionation treatment on the alloy block sample under the conditions that the pressure of the reaction bin is 2MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 3.0X10 -4 And (3) under the Pa vacuum degree and at the temperature of 445-455 ℃, carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) Extracting high trueEmpty: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 3.0X10 -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:6, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches 2MPa working pressure;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 12mins, then continuously raising the temperature to 345-355 ℃ for 12mins, and finally continuously raising the temperature to 445-455 ℃ for 3mins;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: carrying out shot blasting treatment on the sample for 8 hours under the conditions of the reaction bin pressure of 2MPa and the temperature of 445-455 ℃;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 3.0X10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 12mins, then continuously raising the temperature to 345-355 ℃ for 12mins, and finally continuously raising the temperature to 445-455 ℃ for 3mins;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 1h, a high vacuum valve is in an open state in the process, the reaction chamber is continuously vacuumized, and the pressure of the reaction chamber is kept to be 3.0x10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample; the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 45mins.
The heating pipe is a microwave heating pipe.
Example 3
A method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:4, and performing shot blasting and hydrogenation-disproportionation treatment on the alloy block sample under the conditions that the pressure of the reaction bin is 3MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 4.0X10 -4 And (3) under the Pa vacuum degree and at the temperature of 445-455 ℃, carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 4.0X10 -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:4, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches a working pressure of 3 MPa;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 9mins, then continuously raising the temperature to 345-355 ℃ for 9mins, and finally continuously raising the temperature to 445-455 ℃ for 4mins;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: shot blasting is carried out on the sample under the conditions of the reaction bin pressure of 3MPa and the temperature of 445-455 ℃ for 10 hours;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 4.0X10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 9mins, then continuously raising the temperature to 345-355 ℃ for 9mins, and finally continuously raising the temperature to 445-455 ℃ for 4mins;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 2h, a high vacuum valve is in an open state in the process, the reaction chamber is continuously vacuumized, and the pressure of the reaction chamber is kept to be 4.0x10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample; the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 60mins.
The heating pipe is a microwave heating pipe.
Example 4
A method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:5, and performing shot blasting and hydrogenation-disproportionation treatment on the alloy block sample under the conditions that the pressure of the reaction bin is 4MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 5.0X10 -4 And (3) under the Pa vacuum degree and at the temperature of 445-455 ℃, carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 5.0X10 -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:5, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches 4MPa working pressure;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 10min, then continuously raising the temperature to 345-355 ℃ for 10min, and finally continuously raising the temperature to 445-455 ℃ for 2 min;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: carrying out shot blasting treatment on the sample under the conditions of 4MPa of reaction bin pressure and 445-455 ℃ for 6 hours;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 5.0X10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 10min, then continuously raising the temperature to 345-355 ℃ for 10min, and finally continuously raising the temperature to 445-455 ℃ for 2 min;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 3h, a high vacuum valve is in an open state in the process, the reaction chamber is continuously vacuumized, and the pressure of the reaction chamber is kept to be 5.0x10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample; the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 30mins.
The heating pipe is a microwave heating pipe.
Example 5
A method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:3, and performing shot blasting and hydrogenation-disproportionation treatment on the alloy block sample under the conditions that the pressure of the reaction bin is 5MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 6.0X10 -4 And (3) under the Pa vacuum degree and at the temperature of 445-455 ℃, carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve and opening the high vacuum valvePumping the reaction chamber to 6.0X10 g -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:3, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches 5MPa working pressure;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 11mins, then continuously raising the temperature to 345-355 ℃ for 11mins, and finally continuously raising the temperature to 445-455 ℃ for 3mins;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: shot blasting is carried out on the sample under the conditions of the reaction bin pressure of 5MPa and the temperature of 445-455 ℃ for 2 hours;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 6.0X10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 11mins, then continuously raising the temperature to 345-355 ℃ for 11mins, and finally continuously raising the temperature to 445-455 ℃ for 3mins;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 4 hours, a high vacuum valve is in an open state in the process, the reaction chamber is continuously vacuumized, and the pressure of the reaction chamber is kept to be 6.0x10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample; the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 45mins.
The heating pipe is a microwave heating pipe.
Example 6
A method for rapidly nanocrystallizing an alloy surface, comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:6, and performing shot blasting and hydrogenation-disproportionation treatment on the alloy block sample under the conditions that the pressure of the reaction bin is 6MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 7.0X10 -4 And (3) under the Pa vacuum degree and at the temperature of 445-455 ℃, carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample to obtain the surface nano alloy.
The step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 7.0X10 -4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to a flow rate ratio of 1:6, calculating the pressure of the reaction bin to be 1-6 MPa according to an ideal gas state equation, opening a working area ventilation system and a hydrogen monitoring alarm, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches the working pressure of 6 MPa;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 12mins, then continuously raising the temperature to 345-355 ℃ for 12mins, and finally continuously raising the temperature to 445-455 ℃ for 4mins;
e) Shot blasting and hydrogenation-disproportionation (HD) treatment under the conditions of heat preservation and pressure maintaining: shot blasting is carried out on the sample under the conditions of the reaction bin pressure of 6MPa and the temperature of 445-455 ℃ for 12 hours;
f) After the sample shot blasting and hydrogenation-disproportionation (HD) treatment are finished, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 7.0X10 -4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 12mins, then continuously raising the temperature to 345-355 ℃ for 12mins, and finally continuously raising the temperature to 445-455 ℃ for 4mins;
d) Shot peening and dehydrogenation-recombination (DR) treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 6 hours, a high vacuum valve is in an open state in the process, the reaction chamber is continuously vacuumized, and the pressure of the reaction chamber is kept to be 7.0x10 -4 Pa, ensuring that the hydrogen released from the sample is timely discharged out of the reaction bin;
e) After the sample shot blasting and dehydrogenation-recombination (DR) treatment is finished, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) And (5) shutting down.
The alloy block sample is a magnesium alloy block.
The exhaust step is as follows: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to suck the reaction bin to vacuum to accelerate the exhaust.
The sample cooling step specifically comprises the following steps: a cooling water pipe is opened to cool the furnace body and the reaction bin, and a valve on a nitrogen inlet pipe is opened to quench the sample; the shutdown step is as follows: sealing the reaction chamber, and pumping the pressure of the reaction chamber to a vacuum state of 5+/-0.5 Pa.
The method for rapidly nanocrystallizing the alloy surface further comprises a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins to remove oil stains on the surface; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to hydrogenate-dehydrogenate target surface of the sample, polishing to eliminate surface scratches, respectively ultrasonically cleaning with absolute ethanol and propanol for 30min, drying on filter paper, and rapidly transferring the block sample to a reaction bin.
The low-pressure vacuumizing equipment adopts a Roots rotary vane vacuum pump.
The high-pressure vacuumizing equipment adopts a diffusion pump, and a heater of the diffusion pump is turned on to preheat the diffusion pump before the diffusion pump is used, and the preheating time is 60mins.
The heating pipe is a microwave heating pipe.
The above embodiments are merely illustrative of the principles of the present invention and its effects, and are not intended to limit the invention. Modifications and improvements to the above-described embodiments may be made by those skilled in the art without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications and changes which have been accomplished by those skilled in the art without departing from the spirit and technical spirit of the present invention should be covered by the appended claims.
Claims (8)
1. A method for rapidly nanocrystallizing an alloy surface, which is characterized by comprising the following steps:
1) Fixing the alloy block sample on a sample table of a reaction bin, and sealing a bin cover;
2) Shot blasting and hydrogenation-disproportionation treatment: distributing hydrogen and argon to a reaction bin according to the flow rate ratio of 1:3-1:6, and performing shot blasting, hydrogenation and disproportionation treatment on an alloy block sample under the conditions that the pressure of the reaction bin is 1-6 MPa and the temperature is 445-455 ℃;
3) Shot blasting and dehydrogenation-recombination treatment: the pressure in the reaction chamber was 2.0X10 -4 ～7.0×10 -4 Carrying out shot blasting and dehydrogenation-recombination treatment on the alloy block sample at 445-455 ℃ under Pa vacuum degree to obtain the surface nano alloy;
the step 2) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 2.0X10 -4 ～7.0×10 - 4 Pa；
c) Filling hydrogen and argon: opening a hydrogen source and an argon source, distributing hydrogen and argon to a reaction bin according to the flow rate ratio of 1:3-1:6, and closing the hydrogen source and the argon source when the pressure of the reaction bin reaches the working pressure of 1-6 MPa;
d) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 8-12 mins, then continuously raising the temperature to 345-355 ℃ for 8-12 mins, and finally continuously raising the temperature to 445-455 ℃ for 2-4 mins;
e) Shot blasting and hydrogenation-disproportionation treatment under the conditions of heat preservation and pressure maintaining: shot blasting is carried out on the sample under the conditions of the reaction bin pressure of 1-6 MPa and the temperature of 445-455 ℃ for 0.5-12 h;
f) After the sample shot blasting and the hydrogenation-disproportionation treatment are completed, closing a shot blasting system and a heating pipe, and cooling the sample;
g) Exhausting the reaction bin;
h) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging the sample by adopting a polyethylene bag, vacuumizing, and then placing the sample into a vacuum drying oven for preservation;
i) Shutting down;
the step 3) specifically comprises the following steps:
a) And (5) extracting low vacuum: firstly, a cooling water pipe in a reaction bin is opened, then a low vacuum valve is opened, and the pressure of the reaction bin is pumped to a vacuum state of 5+/-0.5 Pa;
b) And (5) extracting high vacuum: closing the low vacuum valve, opening the high vacuum valve, and pumping the pressure of the reaction chamber to 2.0X10 -4 ～7.0×10 - 4 Pa；
c) Heating: closing a cooling water pipe, opening a heating pipe of a reaction bin, firstly raising the temperature of the reaction bin to 145-155 ℃ for 8-12 mins, then continuously raising the temperature to 345-355 ℃ for 8-12 mins, and finally continuously raising the temperature to 445-455 ℃ for 2-4 mins;
d) Shot blasting and dehydrogenation-recombination treatment under the heat preservation condition: shot blasting is carried out on the sample at the temperature of 445-455 ℃ for 0.5-6 h, a high vacuum valve is in an open state in the process, the reaction bin is continuously vacuumized, and the pressure of the reaction bin is kept to be 2.0 multiplied by 10 -4 ～7.0×10 -4 Pa；
e) After the sample shot blasting and dehydrogenation-recombination treatment is completed, closing a shot blasting system and a heating pipe, and cooling the sample;
f) Discharging and packaging: opening an argon source valve, filling argon into a reaction bin to 1 standard atmospheric pressure, opening a bin cover of the reaction bin, taking out a sample, packaging by adopting a polyethylene bag, vacuumizing, and then placing into a vacuum drying oven for preservation;
g) Shutting down;
the alloy block sample is a magnesium alloy block.
2. The method of claim 1, wherein the step of venting comprises: when the temperature of the reaction bin is reduced to below 50 ℃, an exhaust valve of the reaction bin is opened, when the pressure of the reaction bin reaches 150KPa, the exhaust valve of the reaction bin is closed, and a vacuum valve is opened to vacuumize the reaction bin.
3. The method for rapid nanocrystallization of an alloy surface according to claim 1, wherein the sample cooling step comprises the following steps: and (3) opening a cooling water pipe to cool the reaction bin, and opening a valve on a nitrogen inlet pipe to quench the sample.
4. A method for rapid nanocrystallization of an alloy surface according to claim 3, wherein the argon source has a flow rate of 10 to 50KPa.
5. The method for rapid nanocrystallization of an alloy surface according to claim 4, further comprising a pretreatment step of an initial bulk sample, wherein the pretreatment step of the initial bulk sample is as follows: placing an original alloy block sample into absolute ethyl alcohol, and ultrasonically cleaning for 15mins; sequentially using 600-mesh, 1000-mesh, 2000-mesh, 3000-mesh diamond sand paper and magnesia ethanol solution as abrasives to polish the hydrogenation-dehydrogenation target surface of the sample, respectively ultrasonically cleaning the sample with absolute ethanol and propanol for 30min, placing the sample on filter paper for blow-drying, and transferring the block sample to a reaction bin.
6. An apparatus for rapid nanocrystallization of an alloy surface as defined in claim 1, comprising: the device comprises a hydrogen inlet (1), an argon inlet (2), a shot blasting machine (3), an exhaust pipe (4), a vacuum tube, a heating tube (10) and a cooling water pipe (11), wherein a sample (12) is fixed on a sample table (13) of the shot blasting machine (3), a shot outlet (14) of the shot blasting machine (3) faces the sample (12), the shot outlet (14) is fixed with the inner wall of a reaction bin (15) of the shot blasting machine (3), the exhaust pipe (4) is arranged at the upper end of the reaction bin (15), the hydrogen inlet (1) and the argon inlet (2) are arranged on one side wall of the reaction bin (15), the air inlet end of the hydrogen inlet (1) is communicated with a hydrogen source outside the reaction bin (15), the air inlet end of the argon inlet (2) is communicated with an argon source outside the reaction bin (15), one end of the vacuum tube is communicated with the reaction bin (15), the other end of the vacuum tube is communicated with a vacuumizing device, the inner wall of the reaction bin (15) is also fixed with the exhaust pipe (10), the heating tube (10) is used for heating the cooling water pipe (11) is further fixed on the cooling water pipe (11), and a pressure gauge and a thermometer are also fixed in the reaction bin (15).
7. The apparatus for rapid nanocrystallization of an alloy surface of claim 6, wherein the apparatus for rapid nanocrystallization of an alloy surface further comprises: the nitrogen gas intake pipe (9), the storehouse wall of reaction storehouse (15) is run through in nitrogen gas intake pipe (9), the exit end of nitrogen gas intake pipe (9) set up in sample platform (13) below, the exit end of nitrogen gas intake pipe (9) with reaction storehouse (15) inner wall is fixed, the other end and the liquid nitrogen source intercommunication of nitrogen gas intake pipe (9).
8. The apparatus for rapid nanocrystallization of an alloy surface of claim 7, wherein the vacuum tube comprises: one end of the low vacuum tube is communicated with the reaction bin (15), the other end of the low vacuum tube is communicated with the Roots rotary-vane vacuum pump, one end of the high vacuum tube is communicated with the reaction bin (15), the other end of the high vacuum tube is communicated with the diffusion pump, and the low vacuum tube and the high vacuum tube are respectively provided with a low vacuum valve (5) and a high vacuum valve (6).
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| CN201910697212.2A CN110273120B (en) | 2019-07-30 | 2019-07-30 | Method and device for rapidly nanocrystallizing alloy surface |
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