CN103364304A - Hydrogen release testing device and method in material deformation process - Google Patents
Hydrogen release testing device and method in material deformation process Download PDFInfo
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- CN103364304A CN103364304A CN2013102519282A CN201310251928A CN103364304A CN 103364304 A CN103364304 A CN 103364304A CN 2013102519282 A CN2013102519282 A CN 2013102519282A CN 201310251928 A CN201310251928 A CN 201310251928A CN 103364304 A CN103364304 A CN 103364304A
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Abstract
The invention discloses a hydrogen release testing device and method in a material deformation process. The testing device is a four-level vacuum pump system, namely a mechanical pump, a molecular pump, a titanium evaporation absorption pump and an ion pump. The vacuum degree in a vacuum cavity is improved to the greatest degree, and the vacuum degree in the vacuum cavity can be 10<-9> Pascal before a sample stretches, so that a hydrogen release behavior can be measured during the stages of elastic deformation, yield and plastic deformation of the material, and a dependence relationship of hydrogen transfer on the tissue and structure change in the material deformation process is better reflected. The hydrogen release behavior can be measured during the stages of elastic deformation, yield and plastic deformation of the sample material, and a hydrogen release behavior can be measured when the sample material is broken.
Description
Technical field
The present invention relates to rga technical field of measurement and test in the material, especially relate to hydrogen release proving installation and method of testing in the high material deformation process of a kind of measuring accuracy.
Background technology
Safe and efficient storage hydrogen, defeated hydrogen and hydrogenation are the key issues that the Hydrogen Energy scale utilizes.Wherein, high-pressure hydrogen storing and hydrogenation have that device structure is simple, compression hydrogen prepare energy consumption low, fill and the advantages such as mass rate of emission is fast, present most fuel cell cars, hydrogenation stations, fuel cell plant etc. all adopt high pressure (35MPa or 70MPa) Chu Qing/hydrogenation mode.Yet, hydrogen repeatedly fill with the High Pressure Hydrogen system that discharges in, the STRESS VARIATION that is caused by gas and the infringement of hydrogen can cause material property deteriorated or component failure, i.e. Hydrogen Brittleness Phenomena.
The hydrogen embrittlement of metal depends on that external environment condition hydrogen is to the intrusion of metal under the High Pressure Hydrogen environment, its process comprises: gaseous state transportation, physisorption, the hydrogen molecule diffusion in solution, chemisorption, the metal, wherein the slowest hydrogen diffusion process is controlling factor under the room temperature condition.Hydrogen transmission under the ess-strain condition more can embody the hydrogen transport property of material under carrying, distortion and cracking state.
Japanese patent application publication No.: Unexamined Patent 6-103960, the March 6 nineteen ninety-five day for announcing, emit the proving installation of minimum gas when disclosing a kind of distortion, destruction in the material, it comprises: Material Testing Machine, vacuum chamber, vacuum pump, mass spectrometer etc., by the load deflection to vacuum chamber build-in test sample, utilize mass spectrometer can measure the minimum gas that discharges in the material.The weak point of this invention is: the vacuum tightness that vacuum chamber can reach is on the low side (10
-7Pascal), the hydrogen release in the time of can only measuring Materials Fracture is difficult to measure Microamounts of Hydrogen release in the deformation process; Sealing between load bar and vacuum chamber realizes by O-ring seal, and the friction between load bar and O-ring seal will cause minimum gas (mainly comprising hydrogen and methane) to discharge, and the measuring accuracy that causes deformation in the material is brought out hydrogen release is low.
Summary of the invention
The present invention is in order to overcome the hydrogen release can only measure Materials Fracture time the of the prior art, be difficult to measure Microamounts of Hydrogen release in the deformation process, the deficiency that measuring accuracy is low provides hydrogen release proving installation and method of testing in the high material deformation process of a kind of measuring accuracy.
To achieve these goals, the present invention is by the following technical solutions:
Hydrogen release proving installation in a kind of material deformation process comprises vacuum chamber, is located at the bracing frame in the vacuum chamber and the sample inverting chamber that links with vacuum chamber; Be provided with vacuum gate valve between vacuum chamber and the sample inverting chamber, sample inverting chamber one side is provided with the sample switch, and the sample inverting chamber is provided with gland bonnet, is provided with in the sample inverting chamber be used to the upper anchor clamps and the lower clamp that are installed on the bracing frame; Support frame as described above is provided with the upper grip that matches for upper anchor clamps; Be provided with load bar in the described vacuum chamber, the load bar upper end is provided with the lower chuck that matches with lower clamp;
The vacuum chamber below is provided with tensile loading device, and tensile loading device is connected with load transducer; The cavity of resorption wall of vacuum chamber is provided with through hole, and the load bar lower end is passed successively through hole, bellows interior and is connected with load transducer; Corrugated tube is tightly connected with cavity of resorption wall and the load transducer of vacuum chamber respectively; The outer peripheral face of load bar and through-hole wall clearance fit;
Vacuum chamber is provided with vacuum meter, mass spectrometer and ionic pump, is provided with titanium evaporation absorption pump in the ionic pump; Described sample inverting chamber is provided with molecular pump, and molecular pump is connected with mechanical pump;
Computing machine is electrically connected with vacuum meter, mass spectrometer, load transducer and tensile loading device respectively.
In common vacuum chamber, the gas more than 90% is hydrogen, and namely the hydrogen dividing potential drop is near the vacuum chamber internal pressure.
With respect to the background hydrogen dividing potential drop in the vacuum chamber, the increase of hydrogen dividing potential drop is presented as the Microamounts of Hydrogen that discharges in the sample in the process of the test.Background hydrogen dividing potential drop in the vacuum chamber is lower, gets over the Microamounts of Hydrogen that discharges in the energy Measurement accuracy sample, therefore need improve the vacuum tightness of system as far as possible.
The vacuum tightness of Jap.P. (Unexamined Patent 6-103960) device only has 10
-7Pascal.10
-7Pascal's low vacuum can be covered the partial data information that sample discharges hydrogen, therefore, occurs a hydrogen release peak during sample fracture of this invention, and does not find hydrogen release in the sample deformation process.
Proving installation of the present invention adopts the level Four vacuum pump system, and namely mechanical pump, molecular pump, titanium evaporation absorption pump and ionic pump have improved the vacuum tightness in the vacuum chamber to greatest extent, and before sample stretched, the vacuum tightness in the vacuum chamber can reach 10
-9Pascal, thereby the hydrogen release behavior that can measure elastic properties of materials distortion, surrender, plastic period embody the transmission of material deformation Hydrogen better to the dependence of tissue, structural change.
Jap.P. adopts the external load mode, and the motive seal between load bar and vacuum chamber realizes by rubber seal.Because rubber seal has higher hydrogen penetrability, the sealing mode is difficult to realize high vacuum.And the friction between load bar and O-ring seal will cause minimum gas (mainly comprising hydrogen and methane) to discharge, and have a strong impact on the measuring accuracy of deformation in the sample being brought out hydrogen release.
The present invention adopts the internal tension load mode, and the corrugated tube that is provided with flange by two ends is sealed in load bar in the vacuum chamber, and vacuum chamber is provided with the vacuum chamber flange that matches with upper flange, and load transducer is provided with the sensor flange that matches with lower flange; Be provided with the oxygen-free copper O-ring seal between vacuum chamber flange and the upper flange; Be provided with the oxygen-free copper O-ring seal between sensor flange and the lower flange.
Under the effect of tensile loading device, the downward tensile sample of load bar, in the process that stretches, because corrugated tube has elasticity, corrugated tube can produce telescopic variation, but the load that corrugated tube bears is very little, can not emit gas.
Therefore, the present invention both can realize ultrahigh vacuum, can avoid again the air release that friction causes between load bar and vacuum chamber, had effectively improved measuring accuracy.
As preferably, the front fixture block that described upper anchor clamps comprise locating piece, are positioned at the rear fixture block of locating piece bottom, match with rear fixture block; Rear fixture block is provided with 4 screw holes, and front fixture block is provided with 4 screw holes corresponding with the screw hole of rear fixture block; The right flank of locating piece is provided with riser, and riser is provided with the threaded hole that matches for the sample switch; The rectangular bulk of upper grip, the lower surface middle part of upper grip is provided with for the groove that Open Side Down that matches with locating piece, groove runs through between the left surface and right flank of upper grip, the width at slot opening place is less than the width at other position of groove, and the width of riser is greater than the width at slot opening place.
As preferably, the front fixture block that described lower clamp comprises locating piece, is positioned at the rear fixture block of locating piece bottom, matches with rear fixture block; Rear fixture block is provided with 4 screw holes, and front fixture block is provided with 4 screw holes corresponding with the screw hole of rear fixture block; The upper surface middle part of lower chuck is provided with the groove of opening upwards, and groove runs through between the left surface and right flank of lower chuck, and the width at slot opening position is less than the width at other position of groove.
As preferably, support frame as described above comprises flat board, is located at several support bars on the flat board, and the support bar lower end is connected with the cavity of resorption wall of vacuum chamber; Described dull and stereotyped middle part is provided with montant, and described upper grip is positioned at the montant lower end.
As preferably, described sample switch comprises the stainless-steel tube that is connected with the sample inverting chamber, be located at guide rod in the stainless-steel tube, be sheathed on the magnet ring on the stainless-steel tube; One end of the close sample inverting chamber of guide rod is connected with upper anchor clamps by screw thread, and the end away from the sample inverting chamber of guide rod is provided with the ferromagnetism rod iron.
As preferably, the front surface of described rear fixture block is provided with the raised line of several arrangements; The surface relative with rear fixture block of described front fixture block is provided with several grooves corresponding with raised line.
As preferably, the corrugated tube upper end is tightly connected by the cavity of resorption wall of upper flange and vacuum chamber, and the corrugated tube lower end is tightly connected by lower flange and load transducer.
The method of testing of the hydrogen release proving installation in a kind of material deformation process comprises the steps:
(8-1) open vacuum gate valve, utilize mechanical pump to vacuumize 10 minutes to 20 minutes; Molecular pump begins to vacuumize, and vacuum meter detects vacuum tightness, in the vacuum tightness signal input computing machine;
(8-2) reach 10 when vacuum tightness
-4During Pascal, twine the ribbon heater at vacuum chamber, sample inverting chamber, sample switch, ionic pump, corrugated tube and flange, and at ribbon heater outer wrap aluminium foil;
(8-3) toast vacuum chamber, sample inverting chamber, sample switch, ionic pump, corrugated tube and flange in the temperature range of 150 ° of C to 200 ° of C the ribbon heater, and stoving time is 100 hours to 150 hours;
(8-4) reach 10 when vacuum tightness
-5During Pascal, stop baking, take off aluminium foil; Respectively digital vacuum meter, ionic pump, mass spectrometer and titanium evaporation absorption pump are carried out degas operation;
(8-5) reach 10 when vacuum tightness
-6During Pascal, ionic pump is started working, and closes vacuum gate valve, closure molecule pump and mechanical pump;
(8-6) titanium evaporation absorption pump is started working: make Titanium silk preheating 15 minutes, titanium evaporation absorption pump makes Titanium silk evaporation 1 minute;
(8-7) when working time＜64 of titanium evaporation absorption pump minute, repeating step (8-6);
Close titanium evaporation absorption pump, vacuum chamber is cooled to room temperature, and ionic pump continues to vacuumize;
(8-8) reach 10 when vacuum tightness
-9The time, open the gland bonnet of sample inverting chamber, sample is installed on the upper and lower anchor clamps, close gland bonnet; Open mechanical pump and vacuumize, open molecular pump after 10 minutes, vacuumize 30 minutes to 60 minutes;
(8-9) open vacuum gate valve, magnet ring is moved to the left along stainless-steel tube, utilize the attractive force drive guide rod between magnet ring iron and the ferromagnetism rod iron to move to vacuum chamber, guide rod drives upper and lower anchor clamps and sample enters vacuum chamber, the locating piece of upper anchor clamps enters in the groove of upper grip, and the locating piece of lower clamp enters in the groove of lower chuck;
(8-10) when riser contacts with the right flank of upper and lower chuck, stop moving leader, be rotated counterclockwise magnet ring, magnet ring drives guide rod and is rotated counterclockwise, and guide rod separates with riser, and magnet ring is moved right along stainless-steel tube, and guide rod withdraws from vacuum chamber; Close vacuum gate valve, closure molecule pump and mechanical pump;
(8-11) mass spectrometer begins to measure the hydrogen dividing potential drop, and the data transmission that mass spectrometer and load transducer gather is in computing machine;
(8-12) open the test procedure of computing machine, selected rate of straining in test procedure, the computer control tensile loading device carries out stretched operation according to selected rate of straining to sample;
(8-13) after sample fracture, the computer control tensile loading device stops stretched operation, and mass spectrometer continues to detect hydrogen dividing potential drop 20 minutes to 30 minutes.
As preferably, described rate of straining is 0.1 mm/min to 0.5 mm/min.
The present invention has following beneficial effect: (1) can measure the hydrogen release behavior of sample material elastic deformation, surrender, plastic period, the hydrogen release behavior in the time of measuring again the sample material fracture; (2) measuring accuracy is high; (3) dependence of transmitting tissue, structural change for hydrogen in the research material deformation process provides the authentic data basis.
Description of drawings:
Fig. 1 is that sample of the present invention and anchor clamps are installed in a kind of structural representation in the vacuum chamber;
Fig. 2 is a kind of structural representation of upper grip of the present invention and lower chuck;
Fig. 3 is a kind of structural representation of upper anchor clamps of the present invention and lower clamp;
Fig. 4 is a kind of structural representation of corrugated tube of the present invention, load transducer, tensile loading device;
Fig. 5 is a kind of structural representation of upper and lower chuck of the present invention and upper and lower anchor clamps;
Fig. 6 is the another kind of structural representation of upper and lower chuck of the present invention and upper and lower anchor clamps
Fig. 7 is a kind of structural representation of sample of the present invention;
Fig. 8 is test data figure of the present invention;
Fig. 9 is a kind of process flow diagram of embodiments of the invention.
Among the figure: vacuum chamber 1, bracing frame 2, sample inverting chamber 3, vacuum gate valve 4, gland bonnet 5, upper anchor clamps 6, lower clamp 7, upper grip 8, load bar 9, lower chuck 10, corrugated tube 11, upper flange 12, lower flange 13, load transducer 14, tensile loading device 15, vacuum meter 16, mass spectrometer 17, ionic pump 18, titanium evaporation absorption pump 19, molecular pump 20, mechanical pump 21, locating piece 22, rear fixture block 23, front fixture block 24, riser 25, threaded hole 26, groove 27, dull and stereotyped 28, support bar 29, montant 30, stainless-steel tube 31, guide rod 32, magnet ring 33, ferromagnetism rod iron 34, sample 35.
Embodiment
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment as shown in Figure 1 is the hydrogen release proving installation in a kind of material deformation process, comprises vacuum chamber 1, is located at the bracing frame 2 in the vacuum chamber and the sample inverting chamber 3 that links with vacuum chamber; Be provided with vacuum gate valve 4 between vacuum chamber and the sample inverting chamber, sample inverting chamber one side is provided with the sample switch and is connected, and the sample inverting chamber is provided with gland bonnet 5, is provided with in the sample inverting chamber be used to the upper anchor clamps 6 and the lower clamp 7 that are installed on the bracing frame; Bracing frame is provided with the upper grip 8 that matches for upper anchor clamps; Be provided with load bar 9 in the vacuum chamber, the load bar upper end is provided with the lower chuck 10 that matches with lower clamp;
Vacuum chamber is provided with vacuum meter 16, mass spectrometer 17 and ionic pump 18, is provided with titanium evaporation absorption pump 19 in the ionic pump; The sample inverting chamber is provided with molecular pump 20, and molecular pump is connected with mechanical pump 21;
As shown in Figure 4, corrugated tube 11 upper ends are connected with the vacuum chamber flange seal by upper flange 12, and the corrugated tube lower end is tightly connected by lower flange 13 and sensor flange, and load transducer 14 is connected with tensile loading device 15; The cavity of resorption wall of vacuum chamber is provided with through hole, and the load bar lower end is passed successively through hole, bellows interior and is connected with lower flange; The outer peripheral face of load bar and through-hole wall clearance fit;
Computing machine is electrically connected with vacuum meter, mass spectrometer, load transducer and tensile loading device respectively.
Bracing frame comprises flat board 28, is located at 4 support bars 29 on the flat board, and the support bar lower end is connected with the cavity of resorption wall of vacuum chamber; Dull and stereotyped middle part is provided with montant 30, and upper grip is positioned at the montant lower end.
The sample switch comprises the stainless-steel tube 31 that is connected with the sample inverting chamber, be located at guide rod 32 in the stainless-steel tube, be sheathed on the magnet ring 33 on the stainless-steel tube; One end of the close sample inverting chamber of guide rod is connected with upper anchor clamps by screw thread, and the end away from the sample inverting chamber of guide rod is provided with ferromagnetism rod iron 34.
Such as Fig. 3, Fig. 5, shown in Figure 6, the front fixture block 24 that upper anchor clamps comprise locating piece 22, are positioned at the rear fixture block 23 of locating piece bottom, match with rear fixture block; Rear fixture block is provided with 4 screw holes, and front fixture block is provided with 4 screw holes corresponding with the screw hole of rear fixture block; The right flank of locating piece is provided with riser 25, and riser is provided with the threaded hole 26 that matches for the sample switch.
As shown in Figure 2, the rectangular bulk of upper grip, the lower surface middle part of upper grip is provided with for the groove 27 that Open Side Down that matches with locating piece, groove runs through between the left surface and right flank of upper grip, the width at slot opening place is less than the width at other position of groove, and the width of riser is greater than the width at slot opening place.
The front fixture block that lower clamp comprises locating piece, is positioned at the rear fixture block of locating piece bottom, matches with rear fixture block; Rear fixture block is provided with 4 screw holes, and front fixture block is provided with 4 screw holes corresponding with the screw hole of rear fixture block.The front surface of rear fixture block is provided with the raised line of arrangement; The surface relative with rear fixture block of front fixture block is provided with the groove corresponding with raised line.
As shown in Figure 2, the upper surface middle part of lower chuck is provided with the groove of opening upwards, and groove runs through between the left surface and right flank of lower chuck, and the width at slot opening position is less than the width at other position of groove.
As shown in Figure 9, the method for testing of the hydrogen release proving installation in a kind of material deformation process comprises the steps:
Step 100 is opened vacuum gate valve, utilizes mechanical pump to vacuumize 10 minutes to 20 minutes; Molecular pump begins to vacuumize, and vacuum meter detects vacuum tightness, in the vacuum tightness signal input computing machine;
Step 200 is when vacuum tightness reaches 10
-4During Pascal, twine the ribbon heater at vacuum chamber, sample inverting chamber, sample switch, ionic pump, corrugated tube and flange, and at ribbon heater outer wrap aluminium foil;
Step 400 is when vacuum tightness reaches 10
-5During Pascal, stop baking, take off aluminium foil; Respectively digital vacuum meter, ionic pump, mass spectrometer and titanium evaporation absorption pump are carried out degas operation;
Step 500 is when vacuum tightness reaches 10
-6During Pascal, ionic pump is started working, and closes vacuum gate valve, closure molecule pump and mechanical pump;
Step 600, titanium evaporation absorption pump is started working: make Titanium silk preheating 15 minutes, titanium evaporation absorption pump makes Titanium silk evaporation 1 minute;
Step 700, when working time＜64 of titanium evaporation absorption pump minute, repeating step 600;
Close titanium evaporation absorption pump, vacuum chamber is cooled to room temperature, and ionic pump continues to vacuumize;
Step 800 is when vacuum tightness reaches 10
-9The time, open the gland bonnet of sample inverting chamber, as shown in Figure 7 sample 35 is installed on the upper and lower anchor clamps, close gland bonnet; Open mechanical pump and vacuumize, open molecular pump after 10 minutes, vacuumize 30 minutes to 60 minutes;
Step 900, open vacuum gate valve, magnet ring is moved to the left along stainless-steel tube, utilize the attractive force drive guide rod between magnet ring iron and the ferromagnetism rod iron to move to vacuum chamber, guide rod drives upper and lower anchor clamps and sample enters vacuum chamber, the locating piece of upper anchor clamps enters in the groove of upper grip, and the locating piece of lower clamp enters in the groove of lower chuck;
Step 1000 when riser contacts with the right flank of upper and lower chuck, stops moving leader, is rotated counterclockwise magnet ring, and magnet ring drives guide rod and is rotated counterclockwise, and guide rod separates with riser, and magnet ring is moved right along stainless-steel tube, and guide rod withdraws from vacuum chamber; Close vacuum gate valve, closure molecule pump and mechanical pump;
Step 1100, mass spectrometer begin to measure the hydrogen dividing potential drop, and the data transmission that mass spectrometer and load transducer gather is in computing machine;
Step 1200 is opened the test procedure of computing machine, and selected rate of straining is 0.2 mm/min in test procedure, and the computer control tensile loading device carries out stretched operation according to selected rate of straining to sample;
Step 1300, after sample fracture, the computer control tensile loading device stops stretched operation, and mass spectrometer continues to detect hydrogen dividing potential drop 30 minutes.
As shown in Figure 8, wherein a is load and dependent variable relation curve in the 310S stainless steel sample deformation process; Wherein b is the deformation induced hydrogen release curve of 310S stainless steel sample.
In the elastic deformation stage, the hydrogen dividing potential drop increases fast with the increase of load; When reaching yield point, a spike appears in the hydrogen partial pressure curves; Enter plastic period, the hydrogen dividing potential drop increases gradually with the increase of dependent variable, and dependent variable is about 20%, and the hydrogen dividing potential drop reaches maximal value, and the hydrogen dividing potential drop reduces gradually with the increase of dependent variable thereafter; Until during sample fracture, the hydrogen burst size sharply increases, and forms an explosion type hydrogen release peak.
Hydrogen release phenomenon when Jap.P. (Unexamined Patent 6-103960) only can be measured sample fracture can not embody the hydrogen transport behavior in the sample deformation process.
The hydrogen release CLB that proving installation of the present invention is measured reveals the hydrogen transport property under different stress, the strained condition in the sample, especially the sample Dislocations density that causes of deformation is on the impact of hydrogen transport behavior, and to understand the hydrogen transmission significant to the Hydrogen Brittleness Phenomena under the High Pressure Hydrogen environment to deep for this.
Should be understood that the present embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (9)
1. the hydrogen release proving installation in the material deformation process is characterized in that, comprises vacuum chamber (1), is located at the bracing frame (2) in the vacuum chamber and the sample inverting chamber (3) that links with vacuum chamber; Be provided with vacuum gate valve (4) between vacuum chamber and the sample inverting chamber, sample inverting chamber one side is provided with the sample switch, the sample inverting chamber is provided with gland bonnet (5), is provided with in the sample inverting chamber be used to the upper anchor clamps (6) and the lower clamp (7) that are installed on the bracing frame; Support frame as described above is provided with for the upper grip (8) that matches with upper anchor clamps; Be provided with load bar (9) in the described vacuum chamber, the load bar upper end is provided with the lower chuck (10) that matches with lower clamp;
The vacuum chamber below is provided with tensile loading device (15), and tensile loading device is connected with load transducer (14); The cavity of resorption wall of vacuum chamber is provided with through hole, and it is inner and be connected with load transducer that the load bar lower end is passed through hole, corrugated tube (11) successively; Corrugated tube is tightly connected with cavity of resorption wall and the load transducer of vacuum chamber respectively; The outer peripheral face of load bar and through-hole wall clearance fit;
Vacuum chamber is provided with vacuum meter (16), mass spectrometer (17) and ionic pump (18), is provided with titanium evaporation absorption pump (19) in the ionic pump; Described sample inverting chamber is provided with molecular pump (20), and molecular pump is connected with mechanical pump (21);
Computing machine is electrically connected with vacuum meter, mass spectrometer, load transducer and tensile loading device respectively.
2. the hydrogen release proving installation in the material deformation process according to claim 1 is characterized in that, described upper anchor clamps comprise locating piece (22), are positioned at the rear fixture block (23) of locating piece bottom, the front fixture block (24) that matches with rear fixture block; Rear fixture block is provided with 4 screw holes, and front fixture block is provided with 4 screw holes corresponding with the screw hole of rear fixture block; The right flank of locating piece is provided with riser (25), and riser is provided with for the threaded hole (26) that matches with the sample switch; The rectangular bulk of upper grip, the lower surface middle part of upper grip is provided with for the groove that Open Side Down (27) that matches with locating piece, groove runs through between the left surface and right flank of upper grip, the width at slot opening place is less than the width at other position of groove, and the width of riser is greater than the width at slot opening place.
3. the hydrogen release proving installation in the material deformation process according to claim 1 is characterized in that, the front fixture block that described lower clamp comprises locating piece, is positioned at the rear fixture block of locating piece bottom, matches with rear fixture block; Rear fixture block is provided with 4 screw holes, and front fixture block is provided with 4 screw holes corresponding with the screw hole of rear fixture block; The upper surface middle part of lower chuck is provided with the groove of opening upwards, and groove runs through between the left surface and right flank of lower chuck, and the width at slot opening position is less than the width at other position of groove.
4. the hydrogen release proving installation in the material deformation process according to claim 1 is characterized in that, support frame as described above comprises flat board (28), is located at several support bars (29) on the flat board, and the support bar lower end is connected with the cavity of resorption wall of vacuum chamber; Described dull and stereotyped middle part is provided with montant (30), and described upper grip is positioned at the montant lower end.
5. the hydrogen release proving installation in the material deformation process according to claim 1, it is characterized in that, described sample switch comprises the stainless-steel tube (31) that is connected with the sample inverting chamber, be located at guide rod (32) in the stainless-steel tube, be sheathed on the magnet ring (33) on the stainless-steel tube; One end of the close sample inverting chamber of guide rod is connected with upper anchor clamps by screw thread, and the end away from the sample inverting chamber of guide rod is provided with ferromagnetism rod iron (34).
6. according to claim 2 or the hydrogen release proving installation in the 3 described material deformation processes, it is characterized in that, the front surface of described rear fixture block is provided with the raised line of several arrangements; The surface relative with rear fixture block of described front fixture block is provided with several grooves corresponding with raised line.
7. according to claim 1 and 2 or the hydrogen release proving installation in 3 or the 4 or 5 described material deformation processes, it is characterized in that, the corrugated tube upper end is tightly connected by the cavity of resorption wall of upper flange (12) with vacuum chamber, and the corrugated tube lower end is tightly connected by lower flange (13) and load transducer.
8. the method for testing of the hydrogen release proving installation in the material deformation process is characterized in that, comprises the steps:
(8-1) open vacuum gate valve, utilize mechanical pump to vacuumize 10 minutes to 20 minutes; Molecular pump begins to vacuumize, and vacuum meter detects vacuum tightness, in the vacuum tightness signal input computing machine;
(8-2) reach 10 when vacuum tightness
-4During Pascal, twine the ribbon heater at vacuum chamber, sample inverting chamber, sample switch, ionic pump, corrugated tube and flange, and at ribbon heater outer wrap aluminium foil;
(8-3) toast vacuum chamber, sample inverting chamber, sample switch, ionic pump, corrugated tube and flange in the temperature range of 150 ° of C to 200 ° of C the ribbon heater, and stoving time is 100 hours to 150 hours;
(8-4) reach 10 when vacuum tightness
-5During Pascal, stop baking, take off aluminium foil; Respectively digital vacuum meter, ionic pump, mass spectrometer and titanium evaporation absorption pump are carried out degas operation;
(8-5) reach 10 when vacuum tightness
-6During Pascal, ionic pump is started working, and closes vacuum gate valve, closure molecule pump and mechanical pump;
(8-6) titanium evaporation absorption pump is started working: make Titanium silk preheating 15 minutes, titanium evaporation absorption pump makes Titanium silk evaporation 1 minute;
(8-7) when working time＜64 of titanium evaporation absorption pump minute, repeating step (8-6);
Close titanium evaporation absorption pump, vacuum chamber is cooled to room temperature, and ionic pump continues to vacuumize;
(8-8) reach 10 when vacuum tightness
-9The time, open the gland bonnet of sample inverting chamber, sample (35) is installed on the upper and lower anchor clamps, close gland bonnet; Open mechanical pump and vacuumize, open molecular pump after 10 minutes, vacuumize 30 minutes to 60 minutes;
(8-9) open vacuum gate valve, magnet ring is moved to the left along stainless-steel tube, utilize the attractive force drive guide rod between magnet ring iron and the ferromagnetism rod iron to move to vacuum chamber, guide rod drives upper and lower anchor clamps and sample enters vacuum chamber, the locating piece of upper anchor clamps enters in the groove of upper grip, and the locating piece of lower clamp enters in the groove of lower chuck;
(8-10) when riser contacts with the right flank of upper and lower chuck, stop moving leader, be rotated counterclockwise magnet ring, magnet ring drives guide rod and is rotated counterclockwise, and guide rod separates with riser, and magnet ring is moved right along stainless-steel tube, and guide rod withdraws from vacuum chamber; Close vacuum gate valve, closure molecule pump and mechanical pump;
(8-11) mass spectrometer begins to measure the hydrogen dividing potential drop, and the data transmission that mass spectrometer and load transducer gather is in computing machine;
(8-12) open the test procedure of computing machine, selected rate of straining in test procedure, the computer control tensile loading device carries out stretched operation according to selected rate of straining to sample;
(8-13) after sample fracture, the computer control tensile loading device stops stretched operation, and mass spectrometer continues to detect hydrogen dividing potential drop 20 minutes to 30 minutes.
9. the method for testing of the hydrogen release proving installation in the material deformation process according to claim 8 is characterized in that, described rate of straining is 0.1 mm/min to 0.5 mm/min.
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| CN104568727A (en) * | 2014-12-02 | 2015-04-29 | 浙江工业大学 | High temperature and high pressure corrosion hydrogen permeation testing device and method |
| CN108267371A (en) * | 2016-12-30 | 2018-07-10 | 核工业西南物理研究院 | A kind of high temperature and super vacuum small sample tensile creep test device |
| CN110579423A (en) * | 2019-10-18 | 2019-12-17 | 河南理工大学 | Gas desorption experimental system under pressure and temperature changing conditions |
| CN113237756A (en) * | 2021-05-17 | 2021-08-10 | 王丽娜 | Hydrogen embrittlement detector for high-strength steel production |
| CN114624145A (en) * | 2022-05-16 | 2022-06-14 | 上海景瑞阳实业有限公司 | System and method for detecting hydrogen escape rate of metal material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6366839A (en) * | 1986-09-08 | 1988-03-25 | Agency Of Ind Science & Technol | Gas analyzing system for environmental resistance evaluation test |
| JPH06103960A (en) * | 1992-09-16 | 1994-04-15 | Tokyo Univ | Spectrometry for infinitesimal amount of gas emitted from deformed and ruptured material |
| RU2389004C1 (en) * | 2009-01-11 | 2010-05-10 | Физико-технический институт Уральского отделения Российской Академии Наук ФТИ УрО РАН | Device for introduction of sample into vacuum chamber |
| CN101718666A (en) * | 2009-12-17 | 2010-06-02 | 中国航天科技集团公司第五研究院第五一○研究所 | Metal system for testing outgassing property of low-temperature material |
| CN202275069U (en) * | 2011-09-23 | 2012-06-13 | 聚光科技(杭州)股份有限公司 | Sample injection device for mass spectrometry |
| CN202661441U (en) * | 2012-07-06 | 2013-01-09 | 华南师范大学 | Two-beam laser mass spectrometry sample injection system |
-
2013
- 2013-06-21 CN CN201310251928.2A patent/CN103364304B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6366839A (en) * | 1986-09-08 | 1988-03-25 | Agency Of Ind Science & Technol | Gas analyzing system for environmental resistance evaluation test |
| JPH06103960A (en) * | 1992-09-16 | 1994-04-15 | Tokyo Univ | Spectrometry for infinitesimal amount of gas emitted from deformed and ruptured material |
| RU2389004C1 (en) * | 2009-01-11 | 2010-05-10 | Физико-технический институт Уральского отделения Российской Академии Наук ФТИ УрО РАН | Device for introduction of sample into vacuum chamber |
| CN101718666A (en) * | 2009-12-17 | 2010-06-02 | 中国航天科技集团公司第五研究院第五一○研究所 | Metal system for testing outgassing property of low-temperature material |
| CN202275069U (en) * | 2011-09-23 | 2012-06-13 | 聚光科技(杭州)股份有限公司 | Sample injection device for mass spectrometry |
| CN202661441U (en) * | 2012-07-06 | 2013-01-09 | 华南师范大学 | Two-beam laser mass spectrometry sample injection system |
Non-Patent Citations (1)
| Title |
|---|
| 王欲知等: "《真空技术》", 30 June 2007, 北京：北京航空航天大学出版社, article "真空获得", pages: 259~282 * |
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|---|---|---|---|---|
| CN104568727A (en) * | 2014-12-02 | 2015-04-29 | 浙江工业大学 | High temperature and high pressure corrosion hydrogen permeation testing device and method |
| CN104568727B (en) * | 2014-12-02 | 2017-05-17 | 浙江工业大学 | High temperature and high pressure corrosion hydrogen permeation testing device and method |
| CN108267371A (en) * | 2016-12-30 | 2018-07-10 | 核工业西南物理研究院 | A kind of high temperature and super vacuum small sample tensile creep test device |
| CN110579423A (en) * | 2019-10-18 | 2019-12-17 | 河南理工大学 | Gas desorption experimental system under pressure and temperature changing conditions |
| CN113237756A (en) * | 2021-05-17 | 2021-08-10 | 王丽娜 | Hydrogen embrittlement detector for high-strength steel production |
| CN113237756B (en) * | 2021-05-17 | 2022-10-28 | 内蒙古亿利氢田时代技术有限公司 | Hydrogen embrittlement detector for high-strength steel production |
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