CN115772601A - Aluminum-based intermediate alloy second-phase particle extracting agent and method for obtaining second-phase particles - Google Patents
Aluminum-based intermediate alloy second-phase particle extracting agent and method for obtaining second-phase particles Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention provides an aluminum-based intermediate alloy second-phase particle extracting agent and a method for obtaining second-phase particles, wherein the extracting agent comprises the following components in percentage by volume: 0.5-5% of fatty alcohol sulfate aqueous solution, 1-15% of hydrochloric acid, 1-10% of glacial acetic acid, 1-5% of sodium chloride aqueous solution, 1-3% of hydrofluoric acid and the balance of deionized water. The extracting agent for preparing the second-phase particles of the aluminum-based intermediate alloy has the advantages of simple formula, stable reaction and wide adaptation system, can effectively obtain the second-phase particles of the aluminum-based intermediate alloy, can reduce the damage to the second-phase particles of the aluminum-based intermediate alloy, can realize the rapid preparation of the second-phase particles of the aluminum-based intermediate alloy, observe the three-dimensional morphology of the second-phase particles, and can obtain the statistical distribution of the sizes of the second-phase particles in the aluminum-based intermediate alloy.
Description
Technical Field
The invention belongs to the technical field of preparation of second-phase particles of aluminum master alloy, and particularly relates to the field of refining of high-performance aluminum alloy plate strips and aluminum alloy complex castings requiring high-performance aluminum master alloy, in particular to an extracting agent for the second-phase particles of the aluminum master alloy and a method for obtaining the second-phase particles.
Background
The second phase particles in the aluminum-based master alloy are used as an important role for controlling the effect, particularly the refining and deterioration effects, of the aluminum-based master alloy, and need to be observed in size and shape. Therefore, how to obtain and observe the second phase particles in the aluminum-based master alloy is one of the important ways to obtain the efficient grain refiner and the high-quality aluminum-based master alloy.
The current method for obtaining and observing the second phase particles in the aluminum-based master alloy is mainly through metallographic polishing observation. For example, a quantitative analysis method for texture and morphology of an Al-Ti-B intermediate alloy, published in 2018, no. 1 of 'Special casting and non-ferrous alloy', reports a metallographic observation and measurement method for second-phase particles in an Al-Ti-B intermediate alloy, and the two-dimensional morphology of the second-phase particles is mainly observed through metallographic observation. The observation photograph of the second phase particles such as TiCx shown in the report of "fluorescence of C/Ti stoichimetry in TiCx on the grain refinement of Al-Ti-C master alloy" published in "Journal of Materials Science & Technology" 33.2017 is also a two-dimensional metallographic structure photograph. Other related reports adopt high-end equipment such as a transmission electron microscope and a three-dimensional atom probe to observe the three-dimensional morphology of the second-phase particles, and the method has the advantages of complex process, high technical grade requirement, high price and no contribution to the use of production enterprises.
Meanwhile, for the aluminum-based intermediate alloy, the two-dimensional morphology observed by the metallographic phase cannot correctly display the three-dimensional morphology characteristics of the aluminum-based intermediate alloy, such as: the rod-shaped particles are most likely to exhibit a dot shape in two-dimensional texture observation, and the lamellar shape is most likely to exhibit a rod shape. Therefore, it is highly desirable to develop a simple, efficient, and suitable method for obtaining and observing the second phase particles in aluminum-based master alloys.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides an extractant for second-phase particles of an aluminum-based intermediate alloy and a method for obtaining the second-phase particles, which can realize the rapid preparation of the second-phase particles of the aluminum-based intermediate alloy and observe the three-dimensional morphology of the second-phase particles.
The technical scheme adopted by the invention for solving the technical problem is as follows:
an aluminum-based intermediate alloy second-phase particle extracting agent comprises the following components in percentage by volume: 0.5-5% of fatty alcohol sulfate aqueous solution, 1-15% of hydrochloric acid, 1-10% of glacial acetic acid, 1-5% of sodium chloride aqueous solution, 1-3% of hydrofluoric acid and the balance of deionized water. The concentration of the fatty alcohol sulfate aqueous solution is 15-25 g/L, and the concentration of the sodium chloride aqueous solution is 15-25 g/L.
The main functions of the hydrochloric acid, the glacial acetic acid and the hydrofluoric acid in the extracting agent are to react with an aluminum matrix in the aluminum-based intermediate alloy; the fatty alcohol sulfate and the sodium chloride are used for accurately and synergistically regulating the speed uniformity and the reaction balance of the whole reaction process. If the reaction speed is not uniform, sufficient effective particles cannot be obtained; the reaction is not balanced, and the second phase particles can be damaged in effective shapes and even dissolved and disappear. When any one of the fatty alcohol sulfate and the sodium chloride is used alone, uniform and balanced reaction regulation cannot be accurately realized, and further effective second-phase particles cannot be obtained.
The fatty alcohol sulfate is one or more of sodium dodecyl sulfate, potassium dodecyl sulfate and ammonium dodecyl sulfate.
The aluminum-based intermediate alloy is Al-Ti, al-Zr, al-Fe, al-V, al-Mn, al-B, al-Si, al-C, al-Ti-C, al-Ti-B and the like.
Aluminium-based master alloy second phase particles Al 3 Ti，Al 3 Zr，Al 3 Fe，Al 10 V，Al 6 Mn，AlB 2 ，AlB 12 Primary crystal silicon, eutectic crystal silicon, al 4 C 3 ，TiC，TiB 2 And so on.
The invention also provides a method for obtaining the second phase particles of the aluminum-based master alloy, which comprises the following steps:
(1) Slowly adding an extractant which accounts for 1-5 g/L of the extractant into the extractant, and reacting for 10-12 h, wherein hydrofluoric acid in the extractant firstly dissolves oxide skins on the surface of the aluminum alloy, hydrochloric acid and glacial acetic acid react with an aluminum matrix of the aluminum-based intermediate alloy, and second-phase particles of the aluminum-based intermediate alloy are basically preserved as precipitates due to the control of fatty alcohol sulfate and sodium chloride on the reaction speed;
the reaction time is too long, the amount of the precipitated second phase particles increases, but as the reaction time increases, some second phase particles (e.g., tiAl) increase 3 Particles) will dissolve, resulting in a reduction in the number of second phase particles that precipitate.
(2) After the reaction is finished, taking out the large unreacted intermediate alloy residue, and then standing and precipitating for 0.5-2 h;
(3) Slowly pouring out the reaction solution in the beaker under the condition of not influencing the sediment on the bottom layer of the beaker, and then cleaning the reaction solution according to the recovery requirement of the chemical reagent;
(4) Diluting the solution which cannot be cleaned by adopting deionized water, slowly pouring (cleaning according to the recovery requirement of a chemical reagent) the reaction solution diluted by distilled water in the beaker without influencing the sediment at the bottom of the beaker, and repeating the step for three times;
(5) Pouring the solution containing the precipitate into the filter paper of a designed filtration experiment for filtration by adopting qualitative filter paper and a funnel according to the filtration experiment steps;
(6) Drying the filtered precipitate, generally placing the precipitate in a culture dish for airing;
(7) Collecting precipitate particle powder by using a powder collecting test tube, wherein the particle powder is the aluminum-based intermediate alloy second-phase particles;
(8) And observing the precipitate powder by using a scanning electron microscope, and observing the three-dimensional shape of the second-phase particles by using the obtained picture.
The invention has the advantages and positive effects that:
the method can effectively obtain the second-phase particles of the aluminum-based intermediate alloy, reduce the damage to the second-phase particles of the aluminum-based intermediate alloy, realize the rapid preparation of the second-phase particles of the aluminum-based intermediate alloy, observe the three-dimensional morphology of the second-phase particles and obtain the statistical distribution of the sizes of the second-phase particles in the aluminum-based intermediate alloy.
Drawings
FIG. 1 shows TiAl in Al-5Ti Al-based intermediate alloy obtained in example 1 of the present invention 3 SEM photograph of particle morphology;
FIG. 2 is an SEM photograph of primary silicon and eutectic silicon particle morphology in the Al-20Si aluminum-based master alloy obtained in example 2 of the present invention;
FIG. 3 shows TiB in Al-5Ti-1B Al-based intermediate alloy obtained in example 3 2 SEM photograph of particle morphology;
FIG. 4 is a diagram showing TiAl in Al-5Ti-1B aluminum-based intermediate alloy obtained in example 1 3 A statistical distribution of particle sizes;
FIG. 5 is a comparison of different grades assessing the number of second phase particles;
FIG. 6 is a physical representation of the second phase particles collected at the bottom of the beaker after washing in step (4) of example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It is noted that, unless otherwise indicated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
The evaluation method of the present invention:
the invention sets four evaluation grades for the number (R1) of the second-phase particles obtained in a certain time: excellent (a large amount of distinct particle deposition occurred at the bottom of the beaker) as in (a) of fig. 5; good (small significant particle deposition) as in (b) of fig. 5; medium (small amount of particles deposited, no significant particle deposition was seen, but the solution was cloudy) as in (c) of fig. 5; poor (almost no deposition, solution relatively clear) as in (d) of fig. 5.
The reaction speed control degree (R2) reflects the stability degree of the experimental process and simultaneously ensures the safety of the experiment. The specific test method is a excess material weighing method.
The specific calculation formula is as follows:
of the three formulae, M 0 Selecting the initial mass of the sample unreacted from the aluminium-based master alloy
M 1 Reaction t Front side The mass of the left sample after the time is taken out and dried
M 2 Reaction for a certain time t Spacing(s) (≥t Front side +4 hours) of the sample, taken out of the oven dried mass
M 3 Reaction (t) Rear end +t Spacer ) The mass of the left sample after the time is taken out and dried
C 0 Initial reaction speed
C 1 Intermediate reaction rate
t Front side Initial reaction time, generally 4 hours
t Rear end Intermediate reaction times, generally 4 hours
P-evaluation coefficient of degree of control of reaction rate.
Thus, four evaluation levels of the reaction rate control degree (R2) are set based on the reaction rate control degree evaluation coefficient: preferably (P is more than or equal to 1 and less than or equal to 1.5); good (P is more than 1.5 and less than or equal to 2); middle (P is more than 2 and less than or equal to 3); poor (P > 3).
In the following examples, the hydrochloric acid was concentrated hydrochloric acid having a concentration of 12mol/L, the glacial acetic acid was 17.5mol/L, and the hydrofluoric acid was 33.3mol/L.
Example 1
The proportion of the extracting agent is as follows:
the concentration is 20g/L lauryl sodium sulfate (sodium cocoanut alcohol sulfate) aqueous solution, and the volume fraction is 1%;
hydrochloric acid, volume fraction 5%;
glacial acetic acid, volume fraction 1%;
1% of sodium chloride aqueous solution with the concentration of 20 g/L;
hydrofluoric acid, 3% by volume;
the balance being deionized water.
The aluminum-based intermediate alloy is Al-Ti.
A method for obtaining second phase particles of an aluminum-based master alloy comprises the following steps:
(1) Taking 2000ml of the extracting agent, putting the extracting agent into an open beaker with the capacity of 5000ml, taking 6g of Al-10Ti intermediate alloy, slowly putting the intermediate alloy into the extracting agent, and reacting for 10 hours;
(2) After the reaction is finished, taking out the large unreacted intermediate alloy residue, and then standing and precipitating for 1h;
(3) Slowly pouring out the reaction solution in the beaker under the condition of not influencing the sediment on the bottom layer of the beaker, and then cleaning the reaction solution according to the recovery requirement of the chemical reagent;
(4) Diluting the solution which cannot be cleaned by adopting deionized water, slowly pouring off the solution under the condition of not influencing the sediment at the bottom of the beaker, and repeating the step for three times for the reaction solution diluted by distilled water in the beaker; as can be seen in fig. 6 (the second phase particles collected at the bottom of the beaker).
(5) Pouring the solution containing the precipitate into the filter paper of a designed filtration experiment for filtration by adopting qualitative filter paper and a funnel according to the filtration experiment steps;
(6) Drying the filtered precipitate, and placing the precipitate in a culture dish for airing;
(7) Collecting precipitate particle powder by using a powder collecting test tube, wherein the particle powder is the aluminum-based intermediate alloy second-phase particles;
(8) The three-dimensional morphology of the second phase particles can be observed by observing the precipitate powder through a scanning electron microscope to obtain a photograph, and the obtained TiAl can be clearly seen from the photograph as shown in figure 1 3 The three-dimensional morphology of the second phase particles exists in a basically blocky cubic morphology.
(9) The collected powder was subjected to size analysis using a laser particle sizer to obtain a statistical distribution of the second phase particle size, as shown in fig. 4.
The number (R1) of the second phase particles and the reaction rate control degree (R2) are evaluated by the evaluation method of the invention, and the evaluation result is that R1 is excellent; r2: the advantages are excellent.
Example 2
The difference from the embodiment 1 is that the mixture ratio of the extracting agent is as follows: the sodium cocoanut oil alcohol sulfate is 3% in volume fraction, the hydrochloric acid is 6% in volume fraction, the glacial acetic acid is 5% in volume fraction, the sodium chloride is 3% in volume fraction, the hydrofluoric acid is 2% in volume fraction, and the balance is deionized water.
And (1) taking 8gAl-20Si intermediate alloy, slowly putting the intermediate alloy into 2000ml of extracting agent, and reacting for 12 hours. The evaluation result shows that R1 is excellent; r2: is good. The three-dimensional morphology of the obtained lamellar eutectic silicon and hexahedral primary silicon and other second-phase particles can be clearly seen in fig. 2.
Example 3
The difference from the embodiment 1 is that the proportion of the extracting agent is as follows: 5% of sodium cocoanut oil alcohol sulfate, 12% of hydrochloric acid, 9% of glacial acetic acid, 5% of sodium chloride, 1% of hydrofluoric acid and the balance of deionized water.
Step (1), slowly putting 4g of Al-5Ti-1B intermediate alloy into 2000ml of extracting agent, reacting for 10h, and obtaining an evaluation result that R1 is excellent; r2: the advantages are excellent.
The TiB obtained can be clearly seen from FIG. 3 2 The three-dimensional morphology of the second phase particles exists in the form of flaky hexagons.
Comparative example 1
The difference from example 1 is that R1 was good when only 5% by volume aqueous hydrochloric acid was used in the formulation shown in table 1; r2: and (4) poor. The treatment of the oxide skin at the early stage is insufficient, and the reaction speed is suddenly accelerated at the early stage of reaction and cannot be controlled; in addition, the hydrochloric acid concentration in the early stage is too high, and the reaction is violent in the early stage of the reaction.
Comparative example 2
The difference from example 1 is that only 1% by volume of glacial acetic acid in water was used, and the ratio in table 1 was found to be poor in R1; r2: the advantages are excellent. Glacial acetic acid reacts too slowly with aluminum and cannot treat the scale.
Comparative example 3
The difference from example 1 is that only a hydrofluoric acid aqueous solution having a volume fraction of 3% was used, and the evaluation result was R1 difference according to the formulation in table 1; r2: the advantages are excellent. Hydrofluoric acid is added, although scale can be handled, the reaction is too fast and the process is not well controlled.
Comparative example 4
The difference from example 1 is that R1 was evaluated to be good without using sodium cocoyl sulfate and sodium chloride in the formulation shown in table 1; r2: and (4) poor. The hydrochloric acid concentration in the early stage is too high, so that the reaction is violent in the early stage of the reaction, and the dissolution and disappearance of the second-phase particles in the later reaction process are easily caused.
Comparative example 5
The difference from example 1 is that R1 was good according to the formulation shown in table 1 without using sodium chloride; r2: and (4) poor. The hydrochloric acid concentration in the early stage is too high, so that the reaction is violent in the early stage of the reaction, and the dissolution and disappearance of the second-phase particles in the later reaction process are easily caused.
Comparative example 6
The difference from example 1 is that R1 was evaluated to be good without using glacial acetic acid and hydrofluoric acid according to the formulation shown in table 1; r2: in (1). The scale cinder is not enough to be treated in the early stage, and the reaction speed is suddenly accelerated in the early stage of reaction and cannot be controlled.
Comparative example 7
The difference from example 1 is that, without using hydrochloric acid and hydrofluoric acid, the evaluation results were R1 difference according to the compounding ratio of Table 1; r2: the advantages are excellent. The reaction is too slow to effectively capture the second phase particles.
Comparative example 8
The difference from example 1 is that, without using hydrochloric acid and glacial acetic acid, according to the formulation of table 1, the evaluation result is that R1 is poor; r2: the advantages are excellent. The reaction is too slow to effectively capture the second phase particles.
Comparative example 9
The difference from example 1 is that R1 was good as the ratio in table 1 without using hydrofluoric acid; r2: in (1). The scale cinder is not enough to be treated in the early stage, and the reaction speed is suddenly accelerated in the early stage of reaction and cannot be controlled.
Comparative example 10
The difference from example 1 is that, in the formulation shown in Table 1, without using hydrochloric acid, R1 is poor; r2: the advantages are excellent. The reaction is too slow to effectively capture the second phase particles.
Comparative example 11
The difference from example 1 is that R1 was good as a result of evaluation in the formulation shown in table 1 without using glacial acetic acid; r2: in (1). The hydrochloric acid concentration is too high in the early stage, and the reaction is violent in the early stage of the reaction.
TABLE 1
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. An aluminum-based intermediate alloy second-phase particle extracting agent is characterized by comprising the following components in percentage by volume: 0.5-5% of fatty alcohol sulfate aqueous solution, 1-15% of hydrochloric acid, 1-10% of glacial acetic acid, 1-5% of sodium chloride aqueous solution, 1-3% of hydrofluoric acid and the balance of deionized water; the concentration of the fatty alcohol sulfate aqueous solution is 15-25 g/L, and the concentration of the sodium chloride aqueous solution is 15-25 g/L;
the aluminum-based intermediate alloy is Al-Ti, al-Zr, al-Fe, al-V, al-Mn, al-B, al-Si, al-C, al-Ti-C or Al-Ti-B;
the second phase particles are Al 3 Ti，Al 3 Zr，Al 3 Fe，Al 10 V，Al 6 Mn，AlB 2 ，AlB 12 Primary crystal silicon, eutectic crystal silicon, al 4 C 3 TiC or TIB 2 。
2. The extractant of claim 1, wherein the fatty alcohol sulfate is one or more of sodium dodecyl sulfate, potassium dodecyl sulfate, and ammonium dodecyl sulfate.
3. The use method of the extractant according to claim 1 or 2, characterized in that the extractant is slowly added with an aluminum-based master alloy and reacted for 10 to 12 hours; after the reaction is finished, standing and precipitating for 0.5-2 h; slowly pouring out the reaction solution, filtering the precipitate, and drying or airing the filtered precipitate to obtain particle powder, namely the aluminum-based intermediate alloy second-phase particles.
4. The use method of the extractant as claimed in claim 3, wherein the concentration of the aluminum-based master alloy is 1 to 5g/L of the extractant.
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