阅读说明：本技术 一种细化剂及其制备方法和应用 (Refiner and preparation method and application thereof ) 是由 袁名万 李中奎 胡伟 于 2021-09-28 设计创作，主要内容包括：本发明涉及金属加工技术领域,具体而言,涉及一种细化剂及其制备方法和应用。本发明的一种细化剂,包括碳源、钛源和填充剂；所述碳源包括聚乙烯醇和酚醛树脂；以质量百分比计,钛元素的质量为所述细化剂总质量的5％～40％；以质量百分比计,碳元素的质量为所述细化剂总质量的0.5％～5％。本发明的细化剂含有高活性的碳源,在铝及铝合金正常生产熔炼温度下即能与钛反应生成晶粒细化形核所需的TiC,既达到铝钛碳中间合金的功效,又省去了铝钛碳中间合金生产过程中高温熔炼环节,避免了高温烧损,更加环保低耗,成本低廉便于大规模推广使用；并且在使用过程中能防止Ti、V及Zr元素的沉降偏析。(The invention relates to the technical field of metal processing, in particular to a refiner, and a preparation method and application thereof. The refiner comprises a carbon source, a titanium source and a filler; the carbon source comprises polyvinyl alcohol and phenolic resin; the mass of the titanium element is 5 to 40 percent of the total mass of the refiner in percentage by mass; the mass of the carbon element is 0.5-5% of the total mass of the refiner in percentage by mass. The refiner contains a high-activity carbon source, can react with titanium at the normal production and smelting temperature of aluminum and aluminum alloy to generate TiC required for grain refinement and nucleation, achieves the effect of the aluminum-titanium-carbon intermediate alloy, saves a high-temperature smelting link in the production process of the aluminum-titanium-carbon intermediate alloy, avoids high-temperature burning loss, is more environment-friendly and low in consumption, and is low in cost and convenient for large-scale popularization and use; and can prevent the precipitation segregation of Ti, V and Zr elements in the using process.)

1. A refiner, characterized by comprising a carbon source, a titanium source and a filler;

the carbon source comprises polyvinyl alcohol and phenolic resin;

the mass of the titanium element is 5 to 40 percent of the total mass of the refiner in percentage by mass;

the mass of the carbon element is 0.5-5% of the total mass of the refiner in percentage by mass.

2. The refiner of claim 1, wherein the mass of the polyvinyl alcohol is 60-99% of the mass of the carbon source;

preferably, the mass of the polyvinyl alcohol is 60-80% of the mass of the carbon source;

more preferably, the mass of the polyvinyl alcohol is 65% to 70% of the mass of the carbon source.

3. The refiner of claim 1, wherein the carbon source is 8 to 90 parts, the titanium source is 100 to 750 parts, and the filler is 160 to 892 parts by mass.

4. A refining agent according to any one of claims 1 to 3, wherein the titanium source comprises at least one of elemental titanium and potassium fluotitanate.

5. A refining agent according to any one of claims 1 to 3 wherein the filler comprises weighting agents and fluxing agents;

preferably, the weighting agent comprises elemental manganese;

preferably, the particle size of the weighting agent is 0.5 mm-2 mm;

preferably, the flux comprises at least one of a fluoride salt and a chloride salt;

preferably, the chloride salt comprises at least one of potassium fluoride, sodium chloride, calcium chloride, and magnesium chloride;

preferably, the fluoride salt comprises at least one of potassium fluoroaluminate and sodium fluoroaluminate.

6. The refiner of claim 5, wherein the weight gain agent is 50.1-99% of the weight of the filler;

preferably, the weight of the weighting agent is 50.1 to 75% of the weight of the filler.

7. A refining agent according to claim 1, wherein the refining agent is a cake;

preferably, the weight of the block is 50g to 500 g;

preferably, the density of the refiner is greater than 2.6g/cm³。

8. A method of producing a refining agent according to any of claims 1 to 7, comprising the steps of:

mixing the components uniformly, and then carrying out densification treatment.

9. A method of making a refining agent according to claim 8, wherein the densification comprises mechanical compression moulding.

10. Use of a refiner as claimed in any one of claims 1 to 7 for refining aluminium or aluminium alloys.

Technical Field

The invention relates to the technical field of metal processing, in particular to a refiner, and a preparation method and application thereof.

Background

Among many methods for strengthening aluminum and aluminum alloys, grain refinement is the only effective method for improving strength and plasticity. Therefore, since the 30 s of the last century, it has been found that the addition of Ti element to an aluminum melt can refine grains and is applied to production. In the later 50 s, it was found that adding a small amount of B or C element together with Ti element could significantly improve the refining effect. In the early practical application, Ti and B elements are added into an aluminum melt by mixing and pressing titanium powder, potassium fluoborate and a buffer into blocks (called as titanium boron refiner), and then are developed into an added aluminum-titanium-boron intermediate alloy or an aluminum-titanium-carbon intermediate alloy.

However, when the titanium boron additive and the aluminum titanium boron intermediate alloy are used for grain refinement in actual production, obvious sedimentation segregation of titanium and boron element contents exists, and particularly when a certain proportion of scrap returns containing titanium and boron elements are added for cost reduction, the titanium and boron element contents in the aluminum melt are reduced along with time, and great uncertainty is brought to product components. In addition, Zr element is introduced into most of wrought aluminum alloy products (such as 3 series and 7 series) for improving the nucleation of the strengthening phase, and when the Zr element is introduced to exceed 0.15%, the existence of B element can cause the Zr element to generate larger sedimentation segregation, thus seriously affecting the production quality. In order to solve the settlement segregation of the titanium, zirconium and boron elements, practitioners develop an aluminum-titanium-carbon intermediate alloy, the alloy refines crystal grains, has little influence on the settlement segregation of the titanium and zirconium elements, and has an immune effect on elements which influence the refinement of V and Cr. Graphite is used as a carbon source in the production of the aluminum-titanium-carbon intermediate alloy, the graphite and an aluminum melt are difficult to wet and can be added only by adopting high-temperature strong stirring at the temperature of over 1200 ℃, the energy consumption and the burning loss are both large, the production cost is high, and the large-scale use of the aluminum-titanium-carbon intermediate alloy is limited.

In view of the above, the present invention is particularly proposed.

Disclosure of Invention

The invention aims to provide a refiner, which contains a high-activity carbon source, and the refiner can react with titanium at the normal production and smelting temperature of aluminum and aluminum alloy to generate TiC required by grain refinement and nucleation, so that the effect of an aluminum-titanium-carbon intermediate alloy is achieved, a high-temperature smelting link in the production process of the aluminum-titanium-carbon intermediate alloy is omitted, high-temperature burning loss is avoided, the refiner is more environment-friendly and low in consumption, the cost is low, and the refiner is convenient for large-scale popularization and use.

Another object of the present invention is to provide a process for preparing the above refiner, which is simple and easy to carry out.

The invention also aims to provide the application of the refiner in refining aluminum or aluminum alloy.

In order to achieve the above purpose of the present invention, the following technical solutions are adopted:

according to one aspect of the invention, the invention relates to a refiner comprising a carbon source, a titanium source and a filler;

the carbon source comprises polyvinyl alcohol and phenolic resin;

the mass of the titanium element is 5 to 40 percent of the total mass of the refiner in percentage by mass;

the mass of the carbon element is 0.5-5% of the total mass of the refiner in percentage by mass.

Preferably, the mass of the polyvinyl alcohol is 60-99% of the mass of the carbon source.

Preferably, the mass of the polyvinyl alcohol is 60-80% of the mass of the carbon source.

More preferably, the mass of the polyvinyl alcohol is 65% to 70% of the mass of the carbon source.

Preferably, the carbon source is 8 to 90 parts, the titanium source is 100 to 750 parts, and the filler is 160 to 892 parts by mass.

Preferably, the titanium source comprises at least one of elemental titanium and potassium fluotitanate.

Preferably, the filler includes a weighting agent and a fluxing agent.

Preferably, the weight of the weighting agent is 50.1 to 99% of the weight of the filler.

More preferably, the weight of the weighting agent is 50.1% to 75% of the weight of the filler.

Preferably, the weighting agent comprises elemental manganese.

Preferably, the particle size of the weighting agent is 0.5 mm-2 mm.

Preferably, the flux includes at least one of a fluoride salt and a chloride salt.

Preferably, the chloride salt comprises at least one of potassium fluoride, sodium chloride, calcium chloride and magnesium chloride.

Preferably, the fluoride salt comprises at least one of potassium fluoroaluminate and sodium fluoroaluminate.

Preferably, the refiner is a cake.

Preferably, the mass has a weight of 50g to 500 g.

Preferably, the density of the refiner is greater than 2.6g/cm³。

According to another aspect of the invention, the invention also relates to a preparation method of the refiner, which comprises the following steps:

mixing the components uniformly, and then carrying out densification treatment.

Preferably, the densification process comprises mechanical press forming.

According to another aspect, the invention also relates to the use of said refiner for refining aluminium or aluminium alloys.

Compared with the prior art, the invention has the beneficial effects that:

(1) the refiner of the invention contains a high-activity carbon source which can react with titanium at the normal production and smelting temperature of aluminum and aluminum alloy to generate TiC required by grain refinement and nucleation, thereby not only achieving the effect of the aluminum-titanium-carbon intermediate alloy, but also omitting the high-temperature smelting link in the production process of the aluminum-titanium-carbon intermediate alloy, avoiding high-temperature burning loss, being more environment-friendly and low in consumption, having low cost and being convenient for large-scale popularization and use.

(2) The preparation method of the refiner is simple and feasible, and the refiner can be prepared by mixing the raw material components and then carrying out densification treatment.

(3) The refiner can fine aluminum or aluminum alloy well, and further improve the mechanical property of the aluminum or the aluminum alloy. The refiner does not need to be smelted and alloyed at high temperature before use, and can be added and used at normal smelting temperature of aluminum and aluminum alloy; can prevent the elements of Ti, V and Zr from settling and segregating during the use process.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.

FIG. 1 is an external view of a refiner in an example of the present invention;

FIG. 2 is a graph of grains of a blank sample and a 120 minute sample of example 1 of the present invention;

FIG. 3 is a graph of grains of a blank sample and a 120 minute sample of example 2 of the present invention;

FIG. 4 is a graph of grains of a blank sample and a 120 minute sample of example 3 of the present invention;

FIG. 5 is a graph of the grains of the blank and 120 minute samples of comparative example 2 of the present invention;

FIG. 6 is a graph of the grains of the blank and 120 minute samples of comparative example 3 of the present invention;

FIG. 7 is a graph of grains of a blank sample and a 120 minute sample of comparative example 4 of the present invention;

FIG. 8 is a graph of the grains of the blank and 120 minute samples of comparative example 5 of the present invention.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.

According to one aspect of the invention, the invention relates to a refiner comprising a carbon source, a titanium source and a filler;

the carbon source comprises polyvinyl alcohol and phenolic resin;

the mass of the titanium element is 5 to 40 percent of the total mass of the refiner in percentage by mass;

the mass of the carbon element is 0.5-5% of the total mass of the refiner in percentage by mass.

The refiner of the invention contains a high-activity carbon source which can react with titanium at the normal production and smelting temperature (generally 700-760 ℃) of aluminum and aluminum alloy to generate TiC required by grain refinement and nucleation, thereby not only achieving the effect of the aluminum-titanium-carbon intermediate alloy, but also saving the high-temperature smelting link in the production process of the aluminum-titanium-carbon intermediate alloy, avoiding high-temperature burning loss, being more environment-friendly and low in consumption, having low cost and being convenient for large-scale popularization and use.

Although the decomposition temperature of polyvinyl alcohol is lower, compared with phenolic resin, the polyvinyl alcohol is more beneficial to carbon absorption, but the reaction of polyvinyl alcohol used alone is too violent, the carbon burning loss is larger, and the absorption rate is influenced. Therefore, the refiner obtained by the coordination of the aluminum alloy and the aluminum alloy is more beneficial to carbon absorption, and can better obtain the effect of refining the metal aluminum and the aluminum alloy when being used at the normal production and smelting temperature of the aluminum and the aluminum alloy.

In one embodiment, the polyvinyl alcohol has a pyrolysis temperature of 230 ℃.

In one embodiment, the phenolic resin has a pyrolysis temperature of 575 ℃.

In one embodiment, the mass of the titanium element is 5% to 40% of the total mass of the refiner, and may be selected from 5%, 8%, 10%, 12%, 15%, 17%, 20%, 22%, 25%, 27%, 30%, 32%, 35%, 37% or 40%, and other values within the above range may be selected, and is not limited thereto.

In one embodiment, the mass of the carbon element is 0.5% to 5% of the total mass of the refiner, and 0.7%, 1%, 1.2%, 1.5%, 1.7%, 2%, 2.2%, 2.5%, 2.7%, 3%, 3.2%, 3.5%, 3.7%, 4%, 4.2%, 4.5%, or 4.7% may be selected, and other values within the above range may be selected, but are not limited thereto.

After the raw materials of the refiner are composed, the mass of the titanium element is ensured to be 5-40% of the total mass of the refiner, and the mass of the carbon element is 0.5-5% of the total mass of the refiner, so that aluminum or aluminum alloy can be better refined, and the strength and toughness of the aluminum and the aluminum alloy are improved.

Preferably, the mass of the polyvinyl alcohol is 60-99% of the mass of the carbon source.

The mass content of carbon in the polyvinyl alcohol was 54.5%, and the mass content of carbon in the phenol resin was 67.7%; and, the price of polyvinyl alcohol is higher than that of phenolic resin. Therefore, the application can ensure the effect of the refiner in the using process and reduce the cost by limiting the dosage proportion of the refiner and the refiner.

In one embodiment, the mass of the polyvinyl alcohol is 60% to 99% of the mass of the carbon source, and 63%, 65%, 67%, 70%, 72%, 75%, 77%, 80%, 82%, 85%, 87%, 90%, 92%, 95%, or 97% may be selected, and other values within the above range may be selected, but are not limited thereto.

Preferably, the mass of the polyvinyl alcohol is 60-80% of the mass of the carbon source;

more preferably, the mass of the polyvinyl alcohol is 65% to 70% of the mass of the carbon source.

Preferably, the carbon source is 8-90 parts by mass, the titanium source is 100-750 parts by mass, and the filler is 160-892 parts by mass.

In one embodiment, the carbon source is 8 to 90 parts by mass, and may be selected from 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, and 85 parts, and other values within the above range may be selected, and are not limited herein.

In one embodiment, the titanium source is 100 to 750 parts by mass, and may be selected from 150 parts, 220 parts, 450 parts, 480 parts, 500 parts, 520 parts, 550 parts, 570 parts, 600 parts, 620 parts, 650 parts, 680 parts, 700 parts, and 720 parts, or may be selected from other values within the above range, and is not limited thereto.

In one embodiment, the filler is 160 to 892 parts by mass, and may be selected from 220 parts, 250 parts, 270 parts, 300 parts, 320 parts, 350 parts, 370 parts, 400 parts, 420 parts, 450 parts, 470 parts, or 500 parts, or other values within the above range may be selected, and the filler is not limited herein.

Preferably, the titanium source comprises at least one of elemental titanium and potassium fluotitanate.

The titanium source in the invention can be simple substance titanium, can also be potassium fluotitanate, and can also be the combination of the simple substance titanium and the potassium fluotitanate.

Preferably, the filler includes a weighting agent and a fluxing agent.

Preferably, the weighting agent comprises elemental manganese.

The adoption of the weighting agent can increase the density of the refiner and further improve the refining effect of the refiner on metal aluminum or aluminum alloy.

Preferably, the particle size of the weighting agent is 0.5 mm-2 mm.

In one embodiment, the particle size of the weighting agent is 0.5mm to 2mm, and may be selected from 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1.0mm, 1.1mm, 1.2mm, 1.3mm, 1.4mm, 1.5mm, 1.6mm, 1.7mm, 1.8mm, and 1.9mm, and other values within the above range may be selected, but are not limited thereto.

Preferably, the flux includes at least one of a fluoride salt and a chloride salt.

Preferably, the chloride salt comprises at least one of potassium fluoride, sodium chloride, calcium chloride and magnesium chloride.

Preferably, the fluoride salt comprises at least one of potassium fluoroaluminate and sodium fluoroaluminate.

In the invention, the proper amount of the fluxing agent is added, so that the melting point of the aluminum or the aluminum alloy can be effectively reduced, and the refining effect of the obtained refiner on the aluminum or the aluminum alloy can be further improved.

Preferably, the weight of the weighting agent is 50.1 to 99% of the weight of the filler.

In one embodiment, the weight of the weighting agent is 50.1% to 99% of the weight of the filler, and 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, or 98% may be selected, and other values within the above range may be selected, and the weight is not limited herein.

More preferably, the weight of the weighting agent is 50.1% to 75% of the weight of the filler.

Preferably, the refiner is a cake.

Preferably, the mass has a weight of 50g to 500 g.

In one embodiment, the weight of the block is 50g to 500g, and may be 70g, 100g, 120g, 150g, 180g, 200g, 220g, 250g, 270g, 300g, 320g, 350g, 370g, 400g, 420g, 450g, 470g, or 490g, and other values within the above range may be selected, which is not limited herein.

Preferably, the density of the refiner is greater than 2.6g/cm³。

In one embodiment, the density of the refiner is greater than 2.6g/cm³Optionally 2.7g/cm³、2.8g/cm³、2.9g/cm³、3.0g/cm³、3.1g/cm³、3.2g/cm³、3.3g/cm³、3.4g/cm³、3.5g/cm³、3.6g/cm³、3.7g/cm³、3.8g/cm³、3.9g/cm³Or 4.0g/cm³And the like, and other values within the above range may be selected, as a matter of course, and are not limited thereto. In one embodiment, the refiner has a density of 2.6g/cm³～4.0g/cm³。

According to another aspect of the invention, the invention also relates to a preparation method of the refiner, which comprises the following steps:

mixing the components uniformly, and then carrying out densification treatment.

The preparation method of the refiner is simple and feasible, and the refiner is prepared by uniformly mixing the raw material components and then carrying out densification treatment.

Preferably, the densification process comprises mechanical press forming.

The refiner can be obtained by mechanically pressing and molding the mixed raw material components.

According to another aspect, the invention also relates to the use of said refiner for refining aluminium or aluminium alloys.

The refiner can fine aluminum or aluminum alloy well, and further improve the mechanical property of the aluminum or the aluminum alloy. The refiner can be added and used at normal aluminum and aluminum alloy smelting temperature without high-temperature smelting alloying before use.

The present invention will be further explained with reference to specific examples and comparative examples.

The appearance of the refiner in the examples of the invention is shown in FIG. 1.

Example 1

A preparation method of a refiner comprises the following steps:

250g of potassium fluotitanate, 5.5g of polyvinyl alcohol (with the carbon content of 54.5 percent), 2.9g of phenolic resin (with the carbon content of 67.7 percent), 440g of manganese metal with the granularity of 0.5-2 mm and 301.6g of potassium fluoaluminate are physically and uniformly mixed, and the mixed material is pressed into a round cake shape by a press to obtain the titanium carbon refiner.

The density of the refiner is detected to be 3.0g/cm³。

According to the raw material calculation, the mass percent of titanium in the titanium-carbon refiner is 5%, and the mass percent of carbon is 0.5%.

Example 2

A preparation method of a refiner comprises the following steps:

421g of metal titanium powder (the mass content of titanium is 95%), 55g of polyvinyl alcohol (the carbon content is 54.5%), 29g of phenolic resin (the carbon content is 67.7%), 250g of manganese metal with the granularity of 0.5-2 mm and 245g of potassium fluoride are physically and uniformly mixed, and the mixture is pressed into a round cake by a press to obtain the titanium carbon refiner.

The density of the refiner is detected to be 3.5g/cm³。

According to the calculation of raw materials, the titanium carbon refiner contains 40% of titanium and 5% of carbon by mass.

Example 3

A preparation method of a refiner comprises the following steps:

158g of metal titanium powder (the mass content of titanium is 95%), 250g of potassium fluotitanate, 28g of polyvinyl alcohol (the carbon content is 54.5%), 15g of phenolic resin (the carbon content is 67.7%), 329g of metal manganese with the granularity of 0.5-2 mm, 120g of potassium fluoride and 200g of potassium fluoroaluminate are physically and uniformly mixed, and the mixed material is pressed into a round cake shape by a press to obtain the titanium carbon refiner.

The density of the refiner is detected to be 3.5g/cm³。

According to the calculation of raw materials, the titanium carbon refiner contains 20% of titanium and 2.5% of carbon by mass.

Comparative example 1

A refiner has a composition of Al5Ti1B alloy.

Comparative example 2

A preparation method of a refiner comprises the following steps:

250g of potassium fluotitanate, 5g of polyvinyl alcohol (with the carbon content of 54.5 percent), 2g of phenolic resin (with the carbon content of 67.7 percent), 540g of manganese metal with the granularity of 0.5-2 mm and 203g of potassium fluoaluminate are physically and uniformly mixed, and the mixture is pressed into a round cake shape by a press to obtain the titanium carbide refiner.

The density of the refiner is detected to be 3.5g/cm³。

According to the raw material calculation, the mass percent of titanium in the titanium-carbon refiner is 5%, and the mass percent of carbon is 0.4%.

Comparative example 3

A preparation method of a refiner comprises the following steps:

250g of potassium fluotitanate, 76g of polyvinyl alcohol (with the carbon content of 54.5 percent), 20g of phenolic resin (with the carbon content of 67.7 percent), 354g of manganese metal with the granularity of 0.5-2 mm and 300g of potassium fluoride are physically and uniformly mixed, and the mixture is pressed into a round cake by a press to obtain the titanium-carbon refiner.

The density of the refiner is detected to be 3.2g/cm³。

According to the calculation of raw materials, the titanium carbon refiner contains 5% of titanium and 5.5% of carbon by mass.

Comparative example 4

A preparation method of a refiner comprises the following steps:

431g of metal titanium powder (the titanium content is 95 percent), 55g of polyvinyl alcohol (the carbon content is 54.5 percent), 29g of phenolic resin (the carbon content is 67.7 percent), 255g of manganese metal with the granularity of 0.5-2 mm and 230g of potassium fluoroaluminate are physically and uniformly mixed, and the mixture is pressed into a round cake shape by a press to obtain the titanium carbon refiner.

The density of the refiner is detected to be 3.1g/cm³。

According to the raw material calculation, the mass percent of titanium in the titanium-carbon refiner is 41 percent, and the mass percent of carbon is 5 percent.

Comparative example 5

A preparation method of a refiner comprises the following steps:

47g of metal titanium powder (the titanium content is 95%), 55g of polyvinyl alcohol (the carbon content is 54.5%), 29g of phenolic resin (the carbon content is 67.7%), 569g of manganese metal with the granularity of 0.5-2 mm and 300g of potassium fluoroaluminate are physically and uniformly mixed, and the mixed material is pressed into a round cake shape by a press to obtain the titanium carbon refiner.

The density of the refiner is detected to be 3.5g/cm³。

According to the raw material calculation, the mass percent of titanium in the titanium-carbon refiner is 4.5%, and the mass percent of carbon is 5%.

Examples of the experiments

200g of the refiner in the embodiment and the comparative example are respectively put into an aluminum melt containing 0.2 percent of zirconium element and 0.1 percent of vanadium element, the temperature is controlled between 720 ℃ and 750 ℃, samples are taken every 30 minutes, and a direct-reading spectrometer is adopted to detect the contents of Ti, Zr and V.

The blank and 120min sample mean grain sizes in the examples were examined by ring mode. The detection standard is according to GB/T3246.1 organization inspection method for deformed aluminum and aluminum alloy products.

The detection results are as follows:

first, the detection result of the refiner of example 1

The grain patterns of the blank and 120min samples of example 1 are shown in FIG. 2, in which (a1) is the blank and (b1) is the 120min sample. The average grain size of the blank was 960 microns and the average grain size of the 120 minute sample was 170 microns.

The results of measuring the time-dependent changes in the Ti, Zr and V contents of the melt after the addition of the refiner of example 1 are shown in Table 1. As is clear from Table 1, the elements Ti, Zr and V did not undergo significant segregation and sedimentation within 120 min.

Table 1 test results of example 1

Element content	Blank space	30 minutes	60 minutes	90 minutes	120 minutes
						V(wt％)	0.10	0.097	0.090	0.094	0.098
Zr(wt％)	0.20	0.191	0.20	0.192	0.188
						Ti(wt％)	0.001	0.035	0.038	0.033	0.038

Second, the detection result of the refiner of example 2

The grain patterns of the blank and 120min samples of example 2 are shown in FIG. 3, where (a2) is the blank and (b2) is the 120min sample; the average grain size of the blank sample was 880 μm, and the average grain size of the 120-minute sample was 120. mu.m.

The results of measuring the time-dependent changes of Ti, Zr and V contents in the melt after the addition of the refiner of example 2 are shown in Table 2. As is clear from Table 2, no significant segregation and precipitation occurred in the elements Ti, Zr and V within 120 min.

Table 2 test results of example 2

Third, the detection result of the refiner of example 3

The grain patterns of the blank and 120min samples of example 3 are shown in FIG. 4, in which (a3) is the blank and (b3) is the 120min sample; the average grain size of the blank sample was 930 microns and the average grain size of the 120 minute sample was 140 microns.

The results of measuring the time-dependent changes of Ti, Zr and V contents in the melt after the addition of the refiner of example 3 are shown in Table 3. As is clear from Table 3, no significant segregation and precipitation occurred in the elements Ti, Zr and V within 120 min.

Table 3 test results of example 3

Element content	Blank space	30 minutes	60 minutes	90 minutes	120 minutes
						V(wt％)	0.10	0.10	0.093	0.098	0.093
Zr(wt％)	0.20	0.193	0.21	0.189	0.192
						Ti(wt％)	0.0005	0.159	0.163	0.166	0.161

Fourth, the detection result of the refiner of comparative example 1

The results of measuring the time-dependent changes in the Ti, Zr and V contents in the melt after the addition of the refiner of comparative example 1 are shown in Table 4. As is clear from Table 4, the elements Ti, Zr and V segregated and settled significantly within 120 min.

Table 4 test results of example 4

Element content	Blank space	30 minutes	60 minutes	90 minutes	120 minutes
						V(wt％)	0.10	0.092	0.085	0.07	0.071
Zr(wt％)	0.20	0.193	0.182	0.158	0.137
						Ti(wt％)	0.001	0.035	0.038	0.027	0.021

Fifth, the result of examining the refiner of comparative example 2

The grain patterns of the blank and 120min samples of comparative example 2 are shown in fig. 5, in which (a4) is the blank and (b4) is the 120min sample; the average grain size of the blank sample is 900 micrometers, the average grain size of the 120-minute sample is 330 micrometers, the average grain size is larger than the average grain size required by industrial aluminum alloy products, and the refining capability of the refiner in the example is insufficient.

Sixthly, the detection result of the refiner of comparative example 3

The grain patterns of the blank and 120min samples of comparative example 3 are shown in fig. 6, in which (a5) is the blank and (b5) is the 120min sample; the average grain size of the blank sample is 930 microns, the average grain size of the 120-minute sample is 350 microns, the average grain size is larger than the average grain size required by an industrial aluminum alloy product, and the refining capability of the refiner is insufficient.

Seventhly, detection results of the refiner of comparative example 4

The grain patterns of the blank and 120min samples of comparative example 4 are shown in fig. 7, in which (a6) is the blank and (b6) is the 120min sample; the average grain size of the blank sample is 860 microns, the average grain size of the 120-minute sample is 380 microns, the average grain size is larger than the average grain size required by industrial aluminum alloy products, and the refining capability of the refiner in the example is insufficient.

Eighthly, detection results of the refiner of comparative example 5

The grain patterns of the blank and 120min samples of comparative example 5 are shown in fig. 8, in which (a7) is the blank and (b7)4 is the 120min sample; the average grain size of the blank sample is 900 micrometers, the average grain size of the 120-minute sample is 300 micrometers, the average grain size is larger than the average grain size required by industrial aluminum alloy products, and the refining capability of the refiner in the example is insufficient.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.