CN102605200B - Composite zirconium salt for adding zirconium into magnesium alloy and preparation method thereof - Google Patents

Composite zirconium salt for adding zirconium into magnesium alloy and preparation method thereof Download PDF

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CN102605200B
CN102605200B CN201210064960.5A CN201210064960A CN102605200B CN 102605200 B CN102605200 B CN 102605200B CN 201210064960 A CN201210064960 A CN 201210064960A CN 102605200 B CN102605200 B CN 102605200B
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zirconates
compound
zirconium
magnesium alloy
melt
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CN102605200A (en
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宝磊
张志强
乐启炽
崔建忠
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Northeastern University China
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Abstract

The invention belongs to the technical field of metallurgy, and particularly relates to a composite zirconium salt for adding zirconium into magnesium alloy and a preparation method thereof. The composite zirconium salt is based on KZrF5, and contains 53 percent by mass of KZrF5, 20 to 25 percent by mass of LiCl, 5 to 10 percent by mass of CaF2 and 12 to 17 percent by mass of KCl, and theoretically, the Zr content is 21.46 percent. The KZrF5 and the halides are respectively melted, then mixed, heated to 650 DEG C and 680 DEG C, cast onto an iron plate and cooled to room temperature, so that the composite zirconium salt is obtained. The composite zirconium salt is added into magnesium alloy melt with the temperature of 700 DEG C to 730 DEG C batch by batch, and the magnesium alloy melt is sufficiently agitated until the surface of the melt does not spark any more. The preparation method for the composite zirconium salt is simple, the materials are cheap, the price of the finished product is not high, and meanwhile, the yield of zirconium is higher.

Description

A kind of compound zirconates that adds zirconium for magnesium alloy and preparation method thereof
Technical field
The invention belongs to metallurgical technology field, be specifically related to a kind of compound zirconates that adds zirconium for magnesium alloy and preparation method thereof.
Background technology
First Britain Elektron company discloses the thin brilliant effect of zirconium to Mg-Cd and Mg-Cd-Zn magnesium alloy in the nineteen thirty-nine patent that is GB511137 in the patent No., and point out with zirconium can refinement containing the magnesium alloy of Zn, Cd, Ce, Ag, Tl, Th, Cu, Bi, Be, Pb and Ca etc., and for the magnesium alloy containing Al, Si, Sn, Mn, Co, Ni and Sb etc., because of with Zr can form be insoluble to magnesium compound without thinning effect.Meanwhile, because the fusing point solubleness high, in magnesium of zirconium is low, be difficult to realize by direct interpolation metal zirconium form the zirconium alloy of magnesium melt, therefore, the mode of adding zirconium becomes the important research content with zirconium Refining Mg Alloy.In early stage magnesium alloy, Zr adds mainly with zirconium tetrachloride or its mixing salt form greatly, but because of ZrCl 4high volatile volatile, must take some special process to realize, as the patent No. English Patent that is GB511482 in disclosed employing of nineteen thirty-nine by ZrCl 4the mode that the mixture forming with NaCl, KCl and Mg is sealed in MAGNESIUM METAL capsule adds at comparatively high temps (850 ℃), and the English Patent that the patent No. is GB533264 is disclosed ZrCl in nineteen forty-one 4or ZrCl 4with CaF 2mixture be pressed into the cake block mode that density is greater than magnesium melt and slightly under low temperature (780 ℃), adding, the United States Patent (USP) that the patent No. is US2788271 is in disclosed employing of nineteen fifty-seven ZrCl 4, ZrF 4, KCl, BaCl 2composite salt after solidifying with KF consolute is added, and the English Patent that the patent No. is GB681286 disclosed to adopt in Mg-Li alloy in nineteen fifty-two adds ZrCl 4(or ZrBr 4) add Zr with LiCl (or LiBr) mixture mode, to reduce the loss of Li and Zr, but these methods are all difficult to realize industrial application because technique is loaded down with trivial details.Occur with K afterwards 2zrF 6the mode that form adds, but pure K 2zrF 6because reacting too violent, and must add at the high temperature that surpasses 900 ℃, cause magnesium melt scaling loss and iron crucible to dissolve the problems such as serious, occur with KZrF afterwards 5with KCl mixture, or K 2zrF 6, CaZrF 6mode with KCl mixture adds, although can guarantee that when adding q.s in magnesium alloy, Zr reaches 0.7%, facts have proved, it is not suitable for large volume magnesium melt and adds zirconium, and the yield of Zr is very low, only has 5 ~ 10%.
The shortcoming that adds mode for overcoming above-mentioned zirconates, be tending towards afterwards adopting Mg-Zr master alloy to improve the controllability of Zr add-on, and avoid zirconates to add the Inclusion Problem that may cause, developed thus the preparation method of many Mg-Zr master alloys, as US Patent No. 2497530 and the disclosed magnesium metal reduction ZrF that uses of US2497531 4can obtain containing Zr amount at the Mg-Zr of 3 ~ 5% left and right master alloy with the mixture of alkaline earth salt; The patent No. is the disclosed reduction of the English Patent of GB734614 ZrF 4with the mixture of NaCl and KCL, obtain containing Zr amount at more than 20% master alloy; The patent No. is the disclosed reduction of the United States Patent (USP) of US2849311 ZrCl 4with NaCl and KCl mixture, obtain containing Zr amount at more than 23% master alloy; The patent No. is the English Patent of GB857709, Russ P disclosed reduction potassium fluozirconate (KF and ZrF that the United States Patent (USP) that the patent No. is US2970904 and the patent No. are RU2287601 4than being 1 ~ 2) with NaCl, MgCl 2with KCl mixture, to obtain containing Zr, measure the master alloy 25% ~ 45%.
At present, in producing containing Zr Magnesium Alloy Industry, all adopt the Mg-Zr master alloy form of measuring as 25wt% or 30wt% containing Zr to add, but industrial practice shows, master alloy form adds fashionable, and the casting yield of Zr is all very low, guarantee that alloying constituent is qualified, its addition is 3 ~ 4 times that nominal forms, be that casting yield only has 25% ~ 35%, and due to Mg-Zr master alloy complicated process of preparation, market value is very high.With regard to producing ZK60 alloy, the cost of Mg-Zr master alloy just accounts for 30% ~ 40% of production cost, and therefore, the key that reduces the production cost that contains Zr magnesium alloy is to reduce to add the cost of Zr and the casting yield that raising adds Zr technique.
From Historical Development, the original intention that adopts Mg-Zr master alloy is to improve to add the controllability of Zr amount and avoid zirconates to add the fused salt Inclusion Problem that may cause, and simplification adds technique.But, huge advance made due to on-the-spot sample analysis technology, the control of bath composition has not been added the impact of mode, simultaneously, in fact in the melting of industrial production interalloy, use flux to cover with refining and remain inevitable, and for avoiding the sedimentation of master alloy block to cause Zr to sink to the bottom loss, also must adopt loaded down with trivial details suspension to add the molten mode of soaking of stirring.Therefore, compare with the zirconates mode that adds, master alloy adds the advantage of mode not obvious, has increased the weight of on the contrary production cost.
Summary of the invention
For at present adding in master alloy mode the expensive problem that Zr exists containing zirconium magnesium alloy, the invention provides a kind of compound zirconates that adds zirconium for magnesium alloy and preparation method thereof, cheap and casting yield is high.
Compound zirconates of the present invention is with KZrF 5(potassium fluozirconate) is base, is added with LiCl, CaF 2with the composite salt of KCl, by mass percentage, contain 53%KZrF 5, 20 ~ 25%LiCl, 5% ~ 10%CaF 2with 12% ~ 17%KCl, the theoretical Zr content of described compound zirconates is 21.46%.
The preparation method of compound zirconates of the present invention carries out according to following steps:
Composition by compound zirconates, takes the KZrF that quantity is 53% mass percent 5, or take 53% mass percent etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, after 200 ℃ are dried, heat to 550 ~ 560 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 20 ~ 25%LiCl, 5% ~ 10%CaF 2with the halogenide of 12% ~ 17%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 650 ~ 700 ℃, after LiCl melts completely, add wherein CaF 2, be heated to 650 ~ 700 ℃, then add KCl, through being stirred to completely, dissolve, be heated to 650 ℃ of insulations, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat while stirring, when being heated to 650 ~ 680 ℃, be cast to iron plate upper, be cooled to room temperature, collect compound zirconates and be stored in loft drier standby.
The compound zirconates that adopts aforesaid method to prepare is laminar pale solid, must be kept in loft drier standby to prevent deliquescence.
By the method that adopts compound zirconates prepared by aforesaid method to join magnesium alloy, be: by required add-on, take compound zirconates, it is joined to temperature is in batches in the magnesium alloy fused mass of 700 ~ 730 ℃, and fully stirs, until bath surface no longer emits Mars.
Wherein the add-on of compound zirconates is determined according to the industrial requirements of magnesium-alloy material.
Compared with prior art, feature of the present invention and beneficial effect are:
It is to adopt zirconates and halogenide to melt respectively that the inventive method is prepared compound zirconates, and the mode of blending again, can avoid having the KZrF compared with low melting point effectively afterwards 5volatilization loss, avoid the ZrCl that may form simultaneously 4volatilization, can guarantee compound zirconates stable components;
Compound zirconates of the present invention has higher zirconium casting yield, and the zirconium casting yield in magnesium alloy fused mass at least reaches 80%;
Compound zirconates preparation method of the present invention is simple, and raw material is cheap, and finished product price is not high, there is higher zirconium casting yield simultaneously, therefore, compare with adopting Mg-Zr master alloy mode, magnesium alloy fused mass adopts this compound zirconates to add zirconium, can significantly reduce the production cost containing zirconium magnesium alloy;
It is 700 ~ 730 ℃ that compound zirconates of the present invention adds temperature, than what add zirconium in master alloy mode, adds 730 ~ 760 ℃ of temperature much lower, therefore can obviously reduce scaling loss and the erosion action of melt to iron crucible of magnesium alloy;
Compound zirconates of the present invention is not only applicable to add zirconium containing zirconium magnesium alloy, can also add zirconium for aluminium alloy.
Accompanying drawing explanation
Fig. 1 is the typical cast structure comparison diagram that the magnesium alloy in embodiment 1 adds compound zirconates front and back;
A wherein: add the magnesium alloy cast tissue before zirconium; B: add the magnesium alloy cast tissue after zirconium;
Fig. 2 is the typical cast structure comparison diagram that the magnesium alloy in embodiment 2 adds compound zirconates front and back;
A: add the magnesium alloy cast tissue before zirconium; B: add the magnesium alloy cast tissue after zirconium;
Fig. 3 is the typical cast structure comparison diagram that the magnesium alloy in embodiment 3 adds compound zirconates front and back;
A: add the magnesium alloy cast tissue before zirconium; B: add the magnesium alloy cast tissue after zirconium;
Fig. 4 is the typical cast structure comparison diagram that the magnesium alloy in embodiment 4 adds compound zirconates front and back;
A: add the magnesium alloy cast tissue before zirconium; B: add the magnesium alloy cast tissue after zirconium.
Embodiment
The KZrF adopting in the present embodiment 5-, LiCl, CaF 2with KCl be the technical pure level raw material that market is bought.
Embodiment 1
Mass percent by compound zirconates, takes 53% KZrF 5or take 53% mix etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, after 200 ℃ are dried, heat to 550 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 22%LiCl, 8%CaF 2and 17%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 650 ℃, after LiCl melts completely, add wherein CaF 2, be heated to 650 ℃, then add KCl, through being stirred to completely, dissolve, be heated to 650 ℃, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat while stirring, when being heated to 650 ℃, be cast to iron plate upper, be cooled to room temperature, collect and obtain consisting of 53%KZrF 5-, 22%LiCl, 8%CaF 2compound zirconates with 17% KCl, is stored in loft drier standby.
Take 12 grams of the compound zirconates that as mentioned above prepared by method, at 730 ℃, minutes 2 join in 500 grams of magnesium alloy fused mass that consist of Mg-1%Y, and actual Zr content is 0.415%, and its casting yield is 80.5%.
Embodiment 2
By the mass percent of compound zirconates, take the KZrF of 53% quantity 5, or take 53% quantity mix etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, after 200 ℃ are dried, heat to 560 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 22%LiCl, 10%CaF 2and 15%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 700 ℃, after LiCl melts completely, add wherein CaF 2, be heated to 700 ℃, then add KCl, through being stirred to completely, dissolve, be heated to 650 ℃, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat while stirring, when being heated to 680 ℃, be cast to iron plate upper, be cooled to room temperature, collect and obtain consisting of 53%KZrF 5-, 22%LiCl, 10%CaF 2compound zirconates with 15% KCl, is stored in loft drier standby.
Take 15 grams of the compound zirconates that as mentioned above prepared by method, at 720 ℃, minutes 3 batches add in 500 grams of magnesium alloy fused mass that consist of Mg-6%Zn, and actual is 0.554% containing Zr amount, and its casting yield is 86.1%.
Embodiment 3
By the mass percent of compound zirconates, take the KZrF of 53% quantity 5or 53% quantity mix etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, after 200 ℃ are dried, heat to 550 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 23%LiCl, 8%CaF 2and 16%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 680 ℃, after LiCl melts completely, add wherein CaF 2, be heated to 650 ℃, then add KCl, through by mixing to dissolving completely, be heated to 650 ℃ of insulations, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat and stir, when being heated to 670 ℃, being cast to iron plate upper, obtaining consisting of 53%KZrF 5-, 23%LiCl, 8%CaF 2compound zirconates with 16% KCl, is stored in loft drier standby.
Take 15 grams of the compound zirconates that as mentioned above prepared by method, at 730 ℃, minutes 3 batches add in 500 grams of magnesium alloy fused mass that consist of Mg-3.48%Zn-3.23%Cu-0.212%Y, and actual is 0.547% containing Zr amount, and its casting yield is 84.9%.
Embodiment 4
By the mass percent of compound zirconates, take the KZrF of 53% quantity 5, or take 53% quantity mix etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, through 200 ℃ dry, heat to 560 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 23%LiCl, 8%CaF 2and 16%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 650 ℃, after LiCl melts completely, add CaF 2, be heated to 700 ℃, then add KCl, through being stirred to completely, dissolve, be heated to 650 ℃, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat while stirring, when being heated to 650 ℃, be cast to iron plate upper, be cooled to room temperature, collect and obtain consisting of 53%KZrF 5, 23%LiCl, 8%CaF 2compound zirconates with 16% KCl.
Take 15 grams of the compound zirconates that as mentioned above prepared by method, at 730 ℃, minutes 4 batches add in 500 grams of Mg-3Ca melts, and actual is 0.562% containing Zr amount, and its casting yield is 87.3%.
Embodiment 5
By the mass percent of compound zirconates, take the KZrF of 53% quantity 5or 53% quantity mix etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, will after 200 ℃ are dried, heat to 560 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 25%LiCl, 10%CaF 2and 12%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 650 ℃, after LiCl melts completely, add CaF 2, be heated to 700 ℃, then add KCl, through being stirred to completely, dissolve, be heated to 650 ℃, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat while stirring, when being heated to 650 ℃, be cast to iron plate upper, be cooled to room temperature, collect and obtain consisting of 53%KZrF 5, 25%LiCl, 10%CaF 2compound zirconates with 12% KCl.
Take 65 grams of the compound zirconates that as mentioned above prepared by method, at 730 ℃, minutes 4 batches add in 7 kg of pure molten aluminiums, and actual is 0.17% containing Zr amount, and its casting yield is 85.3%.

Claims (4)

1. for magnesium alloy, add a compound zirconates for zirconium, it is characterized in that: with KZrF 5for base, be added with LiCl, CaF 2with the composite salt of KCl, by mass percentage, contain 53%KZrF 5, 20～25%LiCl, 5%～10%CaF 2with 12%～17%KCl, the theoretical Zr content of described compound zirconates is 21.46%.
2. a kind of preparation method who adds the compound zirconates of zirconium for magnesium alloy according to claim 1, is characterized in that carrying out according to following steps:
Composition by compound zirconates, takes the KZrF that quantity is 53% mass percent 5, or take 53% mass percent etc. mole KF and ZrF 4, pour in No. 1 plumbago crucible, after 200 ℃ are dried, heat to 550～560 ℃ of fusings, obtain KZrF 5melt;
Meanwhile, by the mass percent of compound zirconates, weigh 20～25%LiCl, 5%～10%CaF 2with the halogenide of 12%～17%KCl, and through 200 ℃ dry, LiCl is joined in No. 2 plumbago crucibles that are preheated to 300 ℃, and is heated to 650～700 ℃, after LiCl melts completely, add wherein CaF 2, be heated to 650～700 ℃, then add KCl, through being stirred to completely, melt, be heated to 650 ℃ of insulations, obtain mixed halide melt;
Mixed halide melt is blended into and fills KZrF 5in No. 1 plumbago crucible of melt, heat while stirring, when being heated to 650～680 ℃, be cast to iron plate upper, be cooled to room temperature, collect compound zirconates and be stored in loft drier standby.
3. a method that adopts compound zirconates claimed in claim 1 to join magnesium alloy, it is characterized in that: according to required add-on, take compound zirconates, it is joined to temperature is in batches in the magnesium alloy fused mass of 700～730 ℃, and fully stir, until bath surface no longer emits Mars, the casting yield of zirconium is at least 80%.
4. a kind of compound zirconates that adds zirconium for magnesium alloy according to claim 1, is characterized in that: this compound zirconates also adds zirconium for aluminium alloy.
CN201210064960.5A 2012-01-13 2012-01-13 Composite zirconium salt for adding zirconium into magnesium alloy and preparation method thereof Expired - Fee Related CN102605200B (en)

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Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
《Grain refinement behavior of potassium fluozirconate (K2ZrF6) salts mixture introduced into Mg-10Gd-3Y》;Sun M et al.;《JOURNAL OF ALLOYS AND COMPOUNDS》;20100402;第494卷;第427页第2.2部分第1段第4-5行、第433页第5部分第1-4段 *
《添加剂精炼法提高精镁质量的研究》;薛循升等;《轻金属》;19941231(第10期);第33页第3.2.1部分、第34页第6部分第1段 *
Sun M et al..《Grain refinement behavior of potassium fluozirconate (K2ZrF6) salts mixture introduced into Mg-10Gd-3Y》.《JOURNAL OF ALLOYS AND COMPOUNDS》.2010,第494卷第427页第2.2部分第1段第4-5行、第433页第5部分第1-4段.
薛循升等.《添加剂精炼法提高精镁质量的研究》.《轻金属》.1994,(第10期),第33页第3.2.1部分、第34页第6部分第1段.

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