CN104215554B - A kind of quick hydrogen-measuring apparatus of aluminium alloy and survey hydrogen methods - Google Patents
A kind of quick hydrogen-measuring apparatus of aluminium alloy and survey hydrogen methods Download PDFInfo
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Abstract
A kind of quick hydrogen-measuring apparatus of aluminium alloy and survey hydrogen methods, belong to alloy melt and purify and detection technique field.Device, including vavuum pump, is provided with sealing ring between cover plate and vacuum tank；Vavuum pump is connected with vacuum chamber by vacuum pipe, and vacuum relief valve, vacuum regulation valve and vacuum meter are separately positioned on vacuum pipe.Method: start vavuum pump, reaches in making vacuum chamber to set pressure, closes vavuum pump, by vacuum chamber pressure release a to atmospheric pressure state, open cover plate；Melt to be measured is poured in crucible so that it is solidify at one atm；Melt to be measured is poured in another crucible, and puts in vacuum chamber, cover cover plate, start vavuum pump, make melt to be measured solidify under the vacuum condition set；Use densitometer to measure the reference sample density solidified at one atm and the sample density solidified under the vacuum condition set, determine the dnesity index of aluminium alloy melt to be measured, determine the hydrogen content of melt to be measured.
Description
Technical field
The invention belongs to alloy melt purify and detection technique field, particularly relate to a kind of quick hydrogen-measuring apparatus of aluminium alloy and survey hydrogen
Method, is mainly used in the detection of Hydrogen In Molten Aluminum Alloys content.
Background technology
The purification of aluminium alloy melt is to ensure that the key technology of its metallurgical quality, and the hydrogen content reduced in melt is that aluminium alloy melt is clean
The main purpose changed.Aluminium alloy is in fusion process, very sensitive to hydrogen or steam, inevitably absorbs to a certain degree
Hydrogen.If melt is untreated just carries out casting (mold casting or continuously casting), pore, the defect such as loose will be produced,
And the hot tearing of ingot casting or foundry goods may be caused, thus increase percent defective.Therefore, on the one hand, in fusion process, reduce as far as possible
The introducing of hydrogen；On the other hand, before casting, melt is carried out degassing and purifying treatment.According to the mechanism of degasification, degasification method
Absorption and the big class of non-adsorbed degasification two can be divided into.Clean up refer to by aluminum alloy melt directly and adsorbent (as various gases,
Liquid, solid refined agent and filter medium etc.) contact, make the gas in adsorbent and aluminum alloy melt occur physicochemical,
Physics or the effect of machinery, reach the purpose of degasification.The method belonging to adsorption cleaning has: flux method, rotation scavenging etc..
Non-adsorbed degasification refers to disobey and is close in melt add adsorbent, and by certain physical action (such as vacuum, ultrasonic wave etc.), changes
The poised state of metal gas system, so that the method that gas and field trash are separated from aluminum alloy melt.Belong to non-adsorbed
The method purified has: application of vacuum, ultrasonic wave process etc..At present, conventional in enterprise degasification method mainly have flux method,
Rotate scavenging etc., wherein rotate scavenging and be most widely used.
Hydrogen content in melt is measured determining the quality of degassing effect after aluminium alloy melt degassing and purifying treatment.At present
Conventional survey hydrogen methods has inert gas closed cycle detection method, solid electrolyte concentration cell method, Hydrogen In Molten Aluminum Alloys dividing potential drop
The direct method of measurement, solid-state survey hydrogen method and Decompressing Solidification Method etc..Inert gas closed cycle detection method is to utilize a kind of special barrier film
Pump, makes the pure inert gas (generally argon gas or nitrogen) as carrier pass through metal bath, and makes inert gas at aluminium alloy
Do not circulate while melt and instrument pipeline lose along closed-loop path.When the bubble of inert gas is by melt, the hydrogen in metal is just
Can spread in bubble, stop circulation when the concentration in bubble and aluminium alloy melt reaches balance.Follow with thermal-conductivity detector measurement
Hydrogen dividing potential drop in ring gas, converses the hydrogen content in melt according to hydrogen dividing potential drop.Common Telegas type liquid hydrogen meter and
Alscan hydrogen meter belongs to inert gas closed cycle detection method.The advantage of the method is that hydrogen content finding speed is very fast, typically needs
Want 5-15 minute；Additionally precision is higher, reaches 0.01ml/100g Al.The deficiency existed is that equipment cost is high, conduct of popping one's head in
Running stores are fragile, operating cost is high.ALSPEC H hydrogen meter belongs to solid electrolyte concentration cell method, CHAPEL hydrogen meter
Belong to the Hydrogen In Molten Aluminum Alloys dividing potential drop direct method of measurement；Both the above method equally exists deficiency, and i.e. equipment cost is high, popping one's head in belongs to
Fragile in running stores, operating cost is high.Severn Science company of Britain exploitation HYSCAN II hydrogen meter be based on
Quantitatively Decompressing Solidification Method, the method is to put into the bath sample of about 100g in vacuum chamber to solidify, and then analyzes in vacuum chamber
Hydrogen dividing potential drop, so that it is determined that the hydrogen content in aluminium alloy melt.The advantage of the method is that precision is high, easily operates.Exist not
In place of foot: result is had an impact by melt with or without field trash；In aluminium alloy, the steam of Volatile Elements (Mg, Zn) easily disturbs and sentences
Disconnected；Equipment cost is high, maintenance cost is high.The RH-402 type hydrogen meter of LECO company belongs to solid-state and surveys hydrogen method, the master of the method
Wanting advantage is that precision is high, there is problems of equipment cost height, operating cost height, and it is slow to analyze speed, be not suitable for online
Survey hydrogen.
Summary of the invention
The problem existed for prior art, the present invention provides a kind of quick hydrogen-measuring apparatus of aluminium alloy and surveys hydrogen methods, its equipment letter
Singly, easily operating, equipment cost and maintenance cost are low, and measurement result is accurate.
To achieve these goals, the present invention adopts the following technical scheme that, a kind of quick hydrogen-measuring apparatus of aluminium alloy, including vavuum pump,
Vacuum chamber, vacuum meter, vacuum relief valve, vacuum regulation valve and crucible；Described vacuum chamber is made up of cover plate and vacuum tank,
Sealing ring it is provided with between cover plate and vacuum tank；Described vavuum pump is connected with vacuum chamber by vacuum pipe, vacuum pressure release
Valve, vacuum regulation valve and vacuum meter are separately positioned on vacuum pipe.
Described vacuum relief valve, vacuum regulation valve are connected with control panel respectively with vacuum meter.
The survey hydrogen methods of the quick hydrogen-measuring apparatus of aluminium alloy described in employing, comprises the steps:
Step one: start vavuum pump, reaches to set pressure in making vacuum chamber by regulation vacuum regulation valve, is then shut off vacuum
Pump, and by vacuum relief valve by vacuum chamber pressure release a to atmospheric pressure state, then open the cover plate of vacuum chamber；
Step 2: be poured in crucible by aluminium alloy melt to be measured so that it is solidify at one atm, as with reference to sample；
Step 3: aluminium alloy melt to be measured is poured in another crucible, and put in vacuum chamber, cover the lid of vacuum chamber
Plate, starts vavuum pump, makes to solidify, as sample under the aluminium alloy melt to be measured vacuum condition set by step one；
Step 4: according to Archimedes' principle, the reference sample solidified at one atm in employing densitometer determination step two
Density DaDensity D with the sample solidified under the vacuum condition set in step 3v；
Step 5: determine dnesity index D of aluminium alloy melt to be measured according to following formulai:
Step 6: according to dnesity index and the relation curve of hydrogen content of aluminium alloy melt, and the aluminium to be measured determined in step 5
Dnesity index D of alloy melti, i.e. can determine that the hydrogen content of aluminium alloy melt to be measured.
The dnesity index of the aluminium alloy melt described in step 6 and the determination method of the relation curve of hydrogen content, comprise the steps:
Step A: start vavuum pump, reaches to set pressure in making vacuum chamber by regulation vacuum regulation valve, is then shut off vacuum
Pump, and by vacuum relief valve by vacuum chamber pressure release a to atmospheric pressure state, then open the cover plate of vacuum chamber；
Step B: be poured in crucible by aluminium alloy melt so that it is solidify at one atm, as with reference to sample；
Step C: aluminium alloy melt is poured in another crucible, and put in vacuum chamber, cover the cover plate of vacuum chamber,
Start vavuum pump, enable aluminum alloy to solidify, as sample under the vacuum condition that melt is set in step；
Step D: according to Archimedes' principle, uses the close of the reference sample that solidifies at one atm in densitometer determination step B
Degree Da1Density D with the sample solidified under the vacuum condition set in step Cv1；
Step E: determine dnesity index D of aluminium alloy melt according to following formulai1:
Step F: measure the hydrogen content in aluminium alloy melt by hydrogen meter；
Step G: obtained the aluminium alloy melt of different hydro content by melt insulation and degasification, and repeat step A to step F,
Dnesity index and the data of hydrogen content to some group aluminum alloy melts；
Step H: the dnesity index of aluminium alloy melt and the relation curve of hydrogen content can be drawn according to above-mentioned data.
Beneficial effects of the present invention:
The present invention utilizes the principle of decompression solidification the relation curve of the dnesity index Yu hydrogen content by setting up aluminium alloy melt, real
Hydrogen quickly surveyed by the simplest, economic aluminium alloy.The present invention can measure the hydrogen content in aluminium alloy, simultaneously finding speed exactly
Hurry up, minute is only 3～5 minutes, is better than other determinators existing and method.It addition, present device is simple, easily
Operation；Equipment cost and maintenance cost are low, and equipment cost is about the 1/20 to 1/10 of existing equipment, and maintenance cost is existing setting
Standby 1/100；This device is easy to mobile simultaneously, and hydrogen is quantitatively surveyed in the stokehold being suitable for aluminium alloy melt.
Accompanying drawing explanation
Fig. 1 is the structural representation of the quick hydrogen-measuring apparatus of aluminium alloy of the present invention；
Fig. 2 is the dnesity index relation curve with hydrogen content of a certain aluminium copper series alloy that one embodiment of the present of invention is set up
Figure；
In figure, 1-vavuum pump, 2-vacuum pipe, 3-vacuum chamber, 4-cover plate, 5-sealing ring, 6-vacuum tank, 7
-vacuum meter, 8-vacuum relief valve, 9-vacuum regulation valve, 10-control panel, 11-crucible, 12-aluminium alloy melt.
Detailed description of the invention
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
Using a certain aluminium copper series alloy as embodiment, the present invention will be further described.
As it is shown in figure 1, a kind of quick hydrogen-measuring apparatus of aluminium alloy, including vavuum pump 1, vacuum chamber 3, vacuum meter 7, vacuum pressure release
Valve 8, vacuum regulation valve 9 and crucible 11；Described vacuum chamber 3 is made up of cover plate 4 and vacuum tank 6, at cover plate 4 with true
Sealing ring 5 it is provided with between empty 6；Described vavuum pump 1 is connected with vacuum chamber 3 by vacuum pipe 2, vacuum pressure release
Valve 8, vacuum regulation valve 9 and vacuum meter 7 are separately positioned on vacuum pipe 2, and described vacuum relief valve 8, vacuum are adjusted
Joint valve 9 is connected with control panel 10 by cable respectively with vacuum meter 7, plays vacuum monitoring and the effect of regulation, vacuum
Table 7 is used for showing vacuum and feeding back to control panel 10 by cable.
The survey hydrogen methods of the quick hydrogen-measuring apparatus of aluminium alloy described in employing, comprises the steps:
Step one: start vavuum pump 1, is regulated in vacuum regulation valve 9 makes vacuum chamber 3 by control panel 10 and reaches to set pressure
Power, described sets a certain specific absolute pressure that pressure is as 0～200mbar, for the present embodiment, this set pressure as
70mbar, is then shut off vavuum pump 1, and passes through vacuum relief valve 8 by vacuum chamber 3 pressure release to an atmospheric pressure state, then
Open the cover plate 4 of vacuum chamber 3；
Step 2: the aluminium alloy melt to be measured 12 of about 100g is poured in thin-wall stainless steel crucible 11 so that it is in atmosphere,
Solidify the most at one atm, as with reference to sample；
Step 3: the aluminium alloy melt to be measured 12 of about 100g is poured in another thin-wall stainless steel crucible 11, and puts into
In vacuum chamber 3, cover the cover plate 4 of vacuum chamber 3, start vavuum pump 1, make aluminium alloy melt 12 institute in step one to be measured
Solidify under the vacuum condition set, as sample；
Step 4: according to Archimedes' principle, the reference sample solidified at one atm in employing densitometer determination step two
Density DaDensity D with the sample solidified under the vacuum condition set in step 3v；
Step 5: determine dnesity index D of aluminium alloy melt to be measured according to following formulai:
Dnesity index can the number of qualitative reaction Dissolved H in Liquid Al-Si Alloy content, the biggest then hydrogen content of dnesity index is the highest；
Step 6: according to dnesity index and the relation curve of hydrogen content of aluminium alloy melt, and the aluminium to be measured determined in step 5
Dnesity index D of alloy melti, i.e. can determine that the hydrogen content of aluminium alloy melt to be measured, corresponding relation curve and matched curve are such as
Shown in Fig. 2, and the relational expression obtaining matched curve is y=0.035ln (x)+0.288.
The dnesity index of the aluminium alloy melt described in step 6 and the determination method of the relation curve of hydrogen content, comprise the steps:
Step A: start vavuum pump 1, is regulated in vacuum regulation valve 9 makes vacuum chamber 3 by control panel 10 and reaches to set pressure
Power, described sets a certain specific absolute pressure that pressure is as 0～200mbar, for the present embodiment, this set pressure as
70mbar, is then shut off vavuum pump 1, and passes through vacuum relief valve 8 by vacuum chamber 3 pressure release to an atmospheric pressure state, then
Open the cover plate 4 of vacuum chamber 3；
Step B: the aluminium alloy melt 12 of about 100g is poured in thin-wall stainless steel crucible 11 so that it is at an atmospheric pressure
Lower solidification, as with reference to sample；
Step C: the aluminium alloy melt 12 of about 100g is poured in another thin-wall stainless steel crucible 11, and put into true
In empty room 3, cover the cover plate 4 of vacuum chamber 3, start vavuum pump 1, enable aluminum alloy to melt 12 set true in step
Solidify under empty condition, as sample；
Step D: according to Archimedes' principle, uses the close of the reference sample that solidifies at one atm in densitometer determination step B
Degree Da1Density D with the sample solidified under the vacuum condition set in step Cv1；
Step E: determine dnesity index D of aluminium alloy melt according to following formulai1:
Step F: measure the hydrogen content in aluminium alloy melt, for this enforcement by Telegas hydrogen meter or Alscan hydrogen meter
Alloy in example uses Alscan hydrogen meter to measure the hydrogen content in melt；
Step G: obtained the aluminium alloy melt of different hydro content by melt insulation and degasification, and repeat step A to step F,
Dnesity index and the data of hydrogen content to some group aluminum alloy melts；
The hydrogen content that the present embodiment obtains is respectively 0.210,0.166,0.125,0.104 and 0.093 ml/100g Al, right
The dnesity index of the aluminium alloy melt answered is respectively 12.17%, 2.61%, 0.86%, 0.55% and 0.46%；
Step H: the dnesity index of aluminium alloy melt and the relation curve of hydrogen content, corresponding pass can be drawn according to above-mentioned data
It is curve and matched curve as in figure 2 it is shown, and to obtain the relational expression of matched curve be y=0.035ln (x)+0.288.
It should be understood that during the relation curve of the dnesity index Yu hydrogen content that determine aluminium alloy melt, used
Aluminium alloy melt can be the close aluminium alloy melt of composition, but uses the measurement result of aluminium alloy melt to be measured more accurate.
Use the present invention to carry out twice test, obtain dnesity index D of aluminium alloy melt respectivelyiWith corresponding hydrogen content, and
Being verified by Alscan hydrogen meter, result is as shown in table 1.
The hydrogen content comparison sheet that the hydrogen content that table 1 uses the present invention to measure measures with Alscan hydrogen meter
| Dnesity index Di | The present invention measures hydrogen content ml/100g Al | Alscan hydrogen meter measures hydrogen content ml/100g Al |
| 0.72% | 0.115 | 0.110 |
| 6.01% | 0.183 | 0.190 |
Visible, utilize dnesity index D of the aluminium alloy melt that the present invention surveyediWith the dnesity index of the aluminium alloy melt set up with
The hydrogen content that the relation curve of hydrogen content records is the most identical with employing the measured hydrogen content of Alscan hydrogen meter.
Claims (1)
1. use a survey hydrogen methods for the quick hydrogen-measuring apparatus of aluminium alloy, the quick hydrogen-measuring apparatus of described aluminium alloy, including vavuum pump,
Vacuum chamber, vacuum meter, vacuum relief valve, vacuum regulation valve and crucible；Described vacuum chamber is made up of cover plate and vacuum tank,
Sealing ring it is provided with between cover plate and vacuum tank；Described vavuum pump is connected with vacuum chamber by vacuum pipe, vacuum pressure release
Valve, vacuum regulation valve and vacuum meter are separately positioned on vacuum pipe；It is characterized in that, described survey hydrogen methods includes as follows
Step:
Step one: start vavuum pump, reaches to set pressure in making vacuum chamber by regulation vacuum regulation valve, is then shut off vacuum
Pump, and by vacuum relief valve by vacuum chamber pressure release a to atmospheric pressure state, then open the cover plate of vacuum chamber；
Step 2: be poured in crucible by aluminium alloy melt to be measured so that it is solidify at one atm, as with reference to sample；
Step 3: aluminium alloy melt to be measured is poured in another crucible, and put in vacuum chamber, cover the lid of vacuum chamber
Plate, starts vavuum pump, makes to solidify, as sample under the aluminium alloy melt to be measured vacuum condition set by step one；
Step 4: according to Archimedes' principle, the reference sample solidified at one atm in employing densitometer determination step two
Density DaDensity D with the sample solidified under the vacuum condition set in step 3v；
Step 5: determine dnesity index D of aluminium alloy melt to be measured according to following formulai:
Step 6: according to dnesity index and the relation curve of hydrogen content of aluminium alloy melt, and the aluminium to be measured determined in step 5
Dnesity index D of alloy melti, i.e. can determine that the hydrogen content of aluminium alloy melt to be measured；
The dnesity index of described aluminium alloy melt and the determination method of the relation curve of hydrogen content, comprise the steps:
Step A: start vavuum pump, reaches to set pressure in making vacuum chamber by regulation vacuum regulation valve, is then shut off vacuum
Pump, and by vacuum relief valve by vacuum chamber pressure release a to atmospheric pressure state, then open the cover plate of vacuum chamber；
Step B: be poured in crucible by aluminium alloy melt so that it is solidify at one atm, as with reference to sample；
Step C: aluminium alloy melt is poured in another crucible, and put in vacuum chamber, cover the cover plate of vacuum chamber,
Start vavuum pump, enable aluminum alloy to solidify, as sample under the vacuum condition that melt is set in step；
Step D: according to Archimedes' principle, uses the close of the reference sample that solidifies at one atm in densitometer determination step B
Degree Da1Density D with the sample solidified under the vacuum condition set in step Cv1；
Step E: determine dnesity index D of aluminium alloy melt according to following formulai1:
Step F: measure the hydrogen content in aluminium alloy melt by hydrogen meter；
Step G: obtained the aluminium alloy melt of different hydro content by melt insulation and degasification, and repeat step A to step F,
Dnesity index and the data of hydrogen content to some group aluminum alloy melts；
Step H: the dnesity index of aluminium alloy melt and the relation curve of hydrogen content can be drawn according to above-mentioned data.
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| CN109321789A (en) * | 2018-12-26 | 2019-02-12 | 江苏奋杰有色金属制品有限公司 | A kind of aluminium ingot and its production technology of dense internal organization |
| CN109655491B (en) * | 2019-01-15 | 2021-04-30 | 安徽奥特佳科技发展有限公司 | Method for detecting overall quality of defects of air holes and shrinkage cavities of aluminum alloy die castings |
| CN109827962A (en) * | 2019-03-15 | 2019-05-31 | 浙江飞哲工贸有限公司 | A kind of method and apparatus for detecting aluminium alloy melt hydrogen content |
| CN113720731A (en) * | 2021-09-23 | 2021-11-30 | 陕西北方动力有限责任公司 | Detection device for hydrogen content of cast aluminum alloy and use method thereof |
| CN115825371A (en) * | 2022-12-06 | 2023-03-21 | 东北大学 | Device and method for measuring hydrogen content in metal |
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