CN104215554A - Rapid hydrogen measurement device and hydrogen measurement method for aluminium alloy - Google Patents
Rapid hydrogen measurement device and hydrogen measurement method for aluminium alloy Download PDFInfo
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Abstract
The invention discloses rapid hydrogen measurement device and hydrogen measurement method for aluminium alloy, and belongs to the technical field of alloy melt purification and detection. The device comprises a vacuum pump, wherein a sealing ring is arranged between a cover board and a vacuum container; the vacuum pump is communicated with a vacuum chamber through a vacuum pipeline; and a vacuum relief valve, a vacuum degree adjusting valve and a vacuum meter are respectively arranged on the vacuum pipeline. The method comprises the following steps: turning on the vacuum pump, so that the set pressure is reached in the vacuum chamber; turning off the vacuum pump, decompressing the vacuum chamber into an atmospheric pressure state, and opening the cover board; casting to-be-measured melt into a crucible, so that the melt is solidified under an atmospheric pressure; pouring the to-be-measured melt into another crucible, putting into the vacuum chamber, covering the cover board, and turning on the vacuum pump, so that the to-be-measured melt is solidified under the set vacuum condition; and measuring the density of a reference sample solidified under the atmospheric pressure and the density of the sample solidified under the set vacuum condition by adopting a densimeter, determining the density index of the to-be-measured aluminium alloy melt, and determining the hydrogen content of the to-be-measured melt.
Description
Technical field
The invention belongs to alloy melt purification and detection technique field, particularly relate to a kind of aluminium alloy Quick Measuring hydrogen production device and survey hydrogen methods, being mainly used in the detection of Hydrogen In Molten Aluminum Alloys content.
Background technology
The purification of aluminium alloy melt is the gordian technique ensureing its metallurgical quality, and the hydrogen richness reduced in melt is the fundamental purpose of purifying aluminium alloy melt.Aluminium alloy in fusion process, to hydrogen or water vapor very responsive, inevitably absorb hydrogen to a certain degree.Just carry out casting (mold casting or continuous casting) if melt does not add process, pore, the defect such as loose will be produced, and the hot tearing of ingot casting or foundry goods may be caused, thus increase rejection rate.Therefore, on the one hand, in fusion process, reduce the introducing of hydrogen as far as possible; On the other hand, degassing and purifying treatment to be carried out to melt before casting.According to the mechanism of degasification, degasification method can be divided into absorption and the large class of non-adsorbed degasification two.Clean up is referred to and directly to be contacted with adsorbent (as various gas, liquid, solid refined agent and filter medium etc.) by aluminum alloy melt, make the gas in adsorbent and aluminum alloy melt that effect that is physicochemical, physics or machinery occur, reach the object of degasification.The method belonging to adsorption cleaning has: flux method, rotation scavenging etc.Non-adsorbed degasification refers to disobey to be close in melt and adds adsorbent, and by certain physical action (as vacuum, ultrasound wave etc.), changes the equilibrium state of metal gas system, thus makes the method that gas and snotter are separated from aluminum alloy melt.The method belonging to non-adsorbed purification has: application of vacuum, ultrasound wave process etc.At present, degasification method conventional in enterprise mainly contains flux method, rotates scavenging etc., wherein rotates scavenging and is most widely used.
The quality determining degassing effect to be measured to the hydrogen richness in melt after aluminium alloy melt degassing and purifying treatment.Survey hydrogen methods conventional at present has inert gas closed cycle detection method, solid electrolyte concentration cell method, the Hydrogen In Molten Aluminum Alloys dividing potential drop direct method of measurement, solid-state survey hydrogen method and Decompressing Solidification Method etc.Inert gas closed cycle detection method utilizes a kind of special membrane pump, make pure inert gas (being generally argon gas or nitrogen) as carrier by metal bath, and inert gas is not lost along closed-loop path in aluminium alloy melt and instrument pipeline circulate.When the bubble of inert gas is by melt, the hydrogen in metal will spread in bubble, stops circulation when the concentration in bubble and aluminium alloy melt reaches balance.Measure the hydrogen dividing potential drop in recyclegas with thermal-conductivity detector, converse the hydrogen richness in melt according to hydrogen dividing potential drop.The liquid hydrogen meter of common Telegas type and Alscan hydrogen meter belong to inert gas closed cycle detection method.The advantage of the method is that hydrogen richness finding speed is very fast, generally needs 5-15 minute; Precision is higher in addition, reaches 0.01ml/100g Al.Exist deficiency be equipment cost high, pop one's head in fragile as consumables, operating cost is high.ALSPEC H hydrogen meter belongs to solid electrolyte concentration cell method, and CHAPEL hydrogen meter belongs to the Hydrogen In Molten Aluminum Alloys dividing potential drop direct method of measurement; Above two kinds of same Shortcomings of method, namely high, the probe of equipment cost belongs to that consumables are fragile, operating cost is high.The HYSCAN II hydrogen meter of Severn Science company of Britain exploitation is based on quantitative Decompressing Solidification Method, the method is put in vacuum chamber by the bath sample of about 100g to solidify, then analyze the hydrogen dividing potential drop in vacuum chamber, thus determine the hydrogen richness in aluminium alloy melt.The advantage of the method is that precision is high, easily operates.The weak point existed: have impact with or without snotter to result in melt; In aluminium alloy, the steam of Volatile Elements (Mg, Zn) easily disturbs judgement; Equipment cost is high, maintenance cost is high.The RH-402 type hydrogen meter of LECO company belongs to solid-state survey hydrogen method, and the major advantage of the method is that precision is high, and Problems existing is that equipment cost is high, operating cost is high, and analysis speed is slow, is not suitable for surveying hydrogen online.
Summary of the invention
For prior art Problems existing, the invention provides a kind of aluminium alloy Quick Measuring hydrogen production device and survey hydrogen methods, its equipment simply, easily operates, equipment cost and maintenance cost low, and measurement result is accurate.
To achieve these goals, the present invention adopts following technical scheme, and a kind of aluminium alloy Quick Measuring hydrogen production device, comprises vacuum pump, vacuum chamber, vacuum meter, vacuum blowdown valve, vacuum tightness variable valve and crucible; Described vacuum chamber is made up of cover plate and vacuum tank, between cover plate and vacuum tank, be provided with O-ring seal; Described vacuum pump is connected with vacuum chamber by vacuum pipe, and vacuum blowdown valve, vacuum tightness variable valve and vacuum meter are separately positioned on vacuum pipe.
Described vacuum blowdown valve, vacuum tightness variable valve are connected with control panel respectively with vacuum meter.
The survey hydrogen methods of the aluminium alloy Quick Measuring hydrogen production device described in employing, comprises the steps:
Step one: start vacuum pump, by regulating vacuum tightness variable valve to make to reach set pressure in vacuum chamber, then closes vacuum pump, and by vacuum blowdown valve by vacuum chamber pressure release to atmospheric pressure state, then opens the cover plate of vacuum chamber;
Step 2: be poured in crucible by aluminium alloy melt to be measured, makes it solidify at one atm, as reference sample;
Step 3: aluminium alloy melt to be measured is poured in another crucible, and put in vacuum chamber, cover the cover plate of vacuum chamber, start vacuum pump, solidify, as sample under making aluminium alloy melt to be measured vacuum condition set in step one;
Step 4: according to Archimedes' principle, adopts the density D of the reference sample solidified at one atm in densitometer determination step two
awith the density D of the sample solidified under the vacuum condition of setting in step 3
v;
Step 5: the dnesity index D determining aluminium alloy melt to be measured according to following formula
i:
Step 6: according to the dnesity index of aluminium alloy melt and the relation curve of hydrogen richness, and the dnesity index D of the aluminium alloy melt to be measured determined in step 5
i, the hydrogen richness of aluminium alloy melt to be measured can be determined.
The defining method of the dnesity index of the aluminium alloy melt described in step 6 and the relation curve of hydrogen richness, comprises the steps:
Steps A: start vacuum pump, by regulating vacuum tightness variable valve to make to reach set pressure in vacuum chamber, then closes vacuum pump, and by vacuum blowdown valve by vacuum chamber pressure release to atmospheric pressure state, then opens the cover plate of vacuum chamber;
Step B: be poured into by aluminium alloy melt in crucible, makes it solidify at one atm, as reference sample;
Step C: aluminium alloy melt is poured in another crucible, and put in vacuum chamber, cover the cover plate of vacuum chamber, start vacuum pump, solidify, as sample under making aluminium alloy melt vacuum condition set in step;
Step D: according to Archimedes' principle, adopts the density D of the reference sample solidified at one atm in densitometer determination step B
a1with the density D of the sample solidified under the vacuum condition of setting in step C
v1;
Step e: according to the dnesity index D of following formula determination aluminium alloy melt
i1:
Step F: measure the hydrogen richness in aluminium alloy melt by hydrogen meter;
Step G: the aluminium alloy melt being obtained different hydro content by melt insulation and degasification, and repeat steps A to step F, obtain some dnesity index of group aluminum alloy melt and the data of hydrogen richness;
Step H: the dnesity index of aluminium alloy melt and the relation curve of hydrogen richness can be drawn according to above-mentioned data.
Beneficial effect of the present invention:
The present invention utilizes reduces pressure the principle of solidifying and by the relation curve of the dnesity index and hydrogen richness of setting up aluminium alloy melt, realizes simple and easy, economic aluminium alloy Quick Measuring hydrogen.The present invention can measure the hydrogen richness in aluminium alloy exactly, and Simultaneously test speed is fast, and minute is only 3 ~ 5 minutes, is better than other determinators existing and method.In addition, present device simply, easily operates; Equipment cost and maintenance cost low, equipment cost is about 1/20 to 1/10 of existing equipment, and maintenance cost is 1/100 of existing equipment; This device is convenient 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 aluminium alloy Quick Measuring hydrogen production device of the present invention;
Fig. 2 is a certain dnesity index of aluminium copper series alloy set up of one embodiment of the present of invention and the graph of relation of hydrogen richness;
In figure, 1-vacuum pump, 2-vacuum pipe, 3-vacuum chamber, 4-cover plate, 5-O-ring seal, 6-vacuum tank, 7-vacuum meter, 8-vacuum blowdown valve, 9-vacuum tightness variable valve, 10-control panel, 11-crucible, 12-aluminium alloy melt.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Using a certain aluminium copper series alloy as embodiment, the present invention will be further described.
As shown in Figure 1, a kind of aluminium alloy Quick Measuring hydrogen production device, comprises vacuum pump 1, vacuum chamber 3, vacuum meter 7, vacuum blowdown valve 8, vacuum tightness variable valve 9 and crucible 11; Described vacuum chamber 3 is made up of cover plate 4 and vacuum tank 6, is provided with O-ring seal 5 between cover plate 4 and vacuum tank 6; Described vacuum pump 1 is connected with vacuum chamber 3 by vacuum pipe 2, vacuum blowdown valve 8, vacuum tightness variable valve 9 and vacuum meter 7 are separately positioned on vacuum pipe 2, described vacuum blowdown valve 8, vacuum tightness variable valve 9 are connected with control panel 10 respectively by cable with vacuum meter 7, the effect played vacuum tightness monitoring and regulate, vacuum meter 7 is for showing vacuum tightness and feeding back to control panel 10 by cable.
The survey hydrogen methods of the aluminium alloy Quick Measuring hydrogen production device described in employing, comprises the steps:
Step one: start vacuum pump 1, vacuum tightness variable valve 9 is regulated to make to reach set pressure in vacuum chamber 3 by control panel 10, described set pressure is a certain specific absolute pressure of 0 ~ 200mbar, for the present embodiment, this set pressure is 70mbar, then close vacuum pump 1, and by vacuum blowdown valve 8 by vacuum chamber 3 pressure release to atmospheric pressure state, then open the cover plate 4 of vacuum chamber 3;
Step 2: be poured in thin-wall stainless steel crucible 11 by the aluminium alloy melt to be measured 12 of about 100g, make it in atmosphere, namely solidify at one atm, as reference 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 put in vacuum chamber 3, cover the cover plate 4 of vacuum chamber 3, start vacuum pump 1, solidify, as sample under making aluminium alloy melt 12 to be measured vacuum condition set in step one;
Step 4: according to Archimedes' principle, adopts the density D of the reference sample solidified at one atm in densitometer determination step two
awith the density D of the sample solidified under the vacuum condition of setting in step 3
v;
Step 5: the dnesity index D determining aluminium alloy melt to be measured according to following formula
i:
Dnesity index can the number of qualitative reaction Dissolved H in Liquid Al-Si Alloy content, and the larger then hydrogen richness of dnesity index is higher;
Step 6: according to the dnesity index of aluminium alloy melt and the relation curve of hydrogen richness, and the dnesity index D of the aluminium alloy melt to be measured determined in step 5
i, can determine the hydrogen richness of aluminium alloy melt to be measured, as shown in Figure 2, and the relational expression obtaining matched curve is y=0.035ln (x)+0.288 for corresponding relation curve and matched curve.
The defining method of the dnesity index of the aluminium alloy melt described in step 6 and the relation curve of hydrogen richness, comprises the steps:
Steps A: start vacuum pump 1, vacuum tightness variable valve 9 is regulated to make to reach set pressure in vacuum chamber 3 by control panel 10, described set pressure is a certain specific absolute pressure of 0 ~ 200mbar, for the present embodiment, this set pressure is 70mbar, then close vacuum pump 1, and by vacuum blowdown valve 8 by vacuum chamber 3 pressure release to atmospheric pressure state, then open the cover plate 4 of vacuum chamber 3;
Step B: be poured in thin-wall stainless steel crucible 11 by the aluminium alloy melt 12 of about 100g, make it solidify at one atm, as reference sample;
Step C: the aluminium alloy melt 12 of about 100g is poured in another thin-wall stainless steel crucible 11, and put in vacuum chamber 3, cover the cover plate 4 of vacuum chamber 3, start vacuum pump 1, solidify, as sample under making aluminium alloy melt 12 vacuum condition set in step;
Step D: according to Archimedes' principle, adopts the density D of the reference sample solidified at one atm in densitometer determination step B
a1with the density D of the sample solidified under the vacuum condition of setting in step C
v1;
Step e: according to the dnesity index D of following formula determination aluminium alloy melt
i1:
Step F: measured the hydrogen richness in aluminium alloy melt by Telegas hydrogen meter or Alscan hydrogen meter, adopts the hydrogen richness in Alscan hydrogen meter mensuration melt for the alloy in the present embodiment;
Step G: the aluminium alloy melt being obtained different hydro content by melt insulation and degasification, and repeat steps A to step F, obtain some dnesity index of group aluminum alloy melt and the data of hydrogen richness;
The hydrogen richness that the present embodiment obtains is respectively 0.210,0.166,0.125,0.104 and 0.093 ml/100g Al, and the dnesity index of corresponding aluminium alloy melt is respectively 12.17%, 2.61%, 0.86%, 0.55% and 0.46%;
Step H: can draw the dnesity index of aluminium alloy melt and the relation curve of hydrogen richness according to above-mentioned data, as shown in Figure 2, and the relational expression obtaining matched curve is y=0.035ln (x)+0.288 for corresponding relation curve and matched curve.
It should be noted that: in the process of the relation curve of the dnesity index and hydrogen richness of determining aluminium alloy melt, the aluminium alloy melt adopted can be the close aluminium alloy melt of composition, but adopts the measurement result of aluminium alloy melt to be measured more accurate.
Employing invention has been twice test, obtains the dnesity index D of aluminium alloy melt respectively
iwith the hydrogen richness of correspondence, and verified by Alscan hydrogen meter, result is as shown in table 1.
The hydrogen richness that table 1 adopts the present invention to measure and the hydrogen richness comparison sheet that Alscan hydrogen meter measures
| Dnesity index D i | The present invention measures hydrogen richness ml/100g Al | Alscan hydrogen meter measures hydrogen richness ml/100g Al |
| 0.72％ | 0.115 | 0.110 |
| 6.01％ | 0.183 | 0.190 |
Visible, the dnesity index D of the aluminium alloy melt utilizing the present invention to survey
ithe hydrogen richness recorded with the dnesity index of set up aluminium alloy melt and the relation curve of hydrogen richness is very identical with employing Alscan hydrogen richness that hydrogen meter measures.
Claims (4)
1. an aluminium alloy Quick Measuring hydrogen production device, is characterized in that comprising vacuum pump, vacuum chamber, vacuum meter, vacuum blowdown valve, vacuum tightness variable valve and crucible; Described vacuum chamber is made up of cover plate and vacuum tank, between cover plate and vacuum tank, be provided with O-ring seal; Described vacuum pump is connected with vacuum chamber by vacuum pipe, and vacuum blowdown valve, vacuum tightness variable valve and vacuum meter are separately positioned on vacuum pipe.
2. aluminium alloy Quick Measuring hydrogen production device according to claim 1, is characterized in that described vacuum blowdown valve, vacuum tightness variable valve is connected with control panel respectively with vacuum meter.
3. adopt the survey hydrogen methods of aluminium alloy Quick Measuring hydrogen production device according to claim 1, it is characterized in that, comprise the steps:
Step one: start vacuum pump, by regulating vacuum tightness variable valve to make to reach set pressure in vacuum chamber, then closes vacuum pump, and by vacuum blowdown valve by vacuum chamber pressure release to atmospheric pressure state, then opens the cover plate of vacuum chamber;
Step 2: be poured in crucible by aluminium alloy melt to be measured, makes it solidify at one atm, as reference sample;
Step 3: aluminium alloy melt to be measured is poured in another crucible, and put in vacuum chamber, cover the cover plate of vacuum chamber, start vacuum pump, solidify, as sample under making aluminium alloy melt to be measured vacuum condition set in step one;
Step 4: according to Archimedes' principle, adopts the density D of the reference sample solidified at one atm in densitometer determination step two
awith the density D of the sample solidified under the vacuum condition of setting in step 3
v;
Step 5: the dnesity index D determining aluminium alloy melt to be measured according to following formula
i:
Step 6: according to the dnesity index of aluminium alloy melt and the relation curve of hydrogen richness, and the dnesity index D of the aluminium alloy melt to be measured determined in step 5
i, the hydrogen richness of aluminium alloy melt to be measured can be determined.
4. the survey hydrogen methods of employing aluminium alloy Quick Measuring hydrogen production device according to claim 3, is characterized in that the defining method of the dnesity index of the aluminium alloy melt described in step 6 and the relation curve of hydrogen richness, comprises the steps:
Steps A: start vacuum pump, by regulating vacuum tightness variable valve to make to reach set pressure in vacuum chamber, then closes vacuum pump, and by vacuum blowdown valve by vacuum chamber pressure release to atmospheric pressure state, then opens the cover plate of vacuum chamber;
Step B: be poured into by aluminium alloy melt in crucible, makes it solidify at one atm, as reference sample;
Step C: aluminium alloy melt is poured in another crucible, and put in vacuum chamber, cover the cover plate of vacuum chamber, start vacuum pump, solidify, as sample under making aluminium alloy melt vacuum condition set in step;
Step D: according to Archimedes' principle, adopts the density D of the reference sample solidified at one atm in densitometer determination step B
a1with the density D of the sample solidified under the vacuum condition of setting in step C
v1;
Step e: according to the dnesity index D of following formula determination aluminium alloy melt
i1:
Step F: measure the hydrogen richness in aluminium alloy melt by hydrogen meter;
Step G: the aluminium alloy melt being obtained different hydro content by melt insulation and degasification, and repeat steps A to step F, obtain some dnesity index of group aluminum alloy melt and the data of hydrogen richness;
Step H: the dnesity index of aluminium alloy melt and the relation curve of hydrogen richness can be drawn according to above-mentioned data.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109655491A (en) * | 2019-01-15 | 2019-04-19 | 安徽奥特佳科技发展有限公司 | A kind of aluminum alloy die casting stomata and shrinkage cavity defect overall quality detection method |
| 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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| 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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