CN107619972A - A kind of manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy - Google Patents
A kind of manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy Download PDFInfo
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- CN107619972A CN107619972A CN201711096566.9A CN201711096566A CN107619972A CN 107619972 A CN107619972 A CN 107619972A CN 201711096566 A CN201711096566 A CN 201711096566A CN 107619972 A CN107619972 A CN 107619972A
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Abstract
The present invention relates to a kind of manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy, manufacture method is in two steps, the first step first prepares aluminium neodymium intermediate alloy using aluminium and neodymium as raw material, second step prepares aluminium neodymium alloy using aluminium and aluminium neodymium intermediate alloy as raw material again, because aluminium neodymium intermediate alloy fusing point is low, proportion is low, purity is high, more matched with the physicochemical property of aluminium, therefore both have preferably to coordinate in fusion process and acted synergistically, fusing time can be shortened, the problems such as overcoming splashing and segregation, reduce pollution, and improve aluminium neodymium alloy purity, reduce impurity content, it can reach 99.999% by aluminium neodymium alloy purity produced by the present invention, so as to which aluminium neodymium alloy quality gets a promotion.
Description
Technical field
The present invention relates to magnetic control spattering target manufacturing field, more particularly to a kind of system of magnetic controlled sputtering target timber-used aluminium neodymium alloy
Make method.
Background technology
Magnetron sputtering plating is a kind of new physical vapor plated film mode, be exactly with electron gun system electron emission simultaneously
Focus on plated material, its atom for being sputtered out is followed momentum transfer principle and flown with higher kinetic energy disengaging material
To substrate deposition film forming.This plated material is just magnetic control spattering target.In order to improve sputtering yield and ensure deposition film
Quality, target quality must be controlled strictly, be shown through a large amount of practical studies, influence target quality principal element include purity,
Impurity content, density, crystallite dimension and Size Distribution, crystalline orientation and structural homogeneity, geometry and size etc., are especially used
In industries such as FPD, energy-conservation low emissivity glass, LED, semiconductor components and devices, very tight is required to purity and impurity content
Lattice.
Aluminium neodymium alloy is a kind of conventional magnetic control spattering target, and the fusing point of aluminium is 660 DEG C, density 2.7, thermal conductivity factor are
0.53, the fusing point of neodymium is 1024 DEG C, density 7.0, thermal conductivity factor 0.031, due to both fusing points, density and thermal conductivity factor
Larger difference be present, if directly taking vacuum melting, it is easy to segregation is produced in fusion process and is splashed, is polluted,
Cause inhomogeneities and the impurity content of alloy structure higher, have a strong impact on alloy mass.
The content of the invention
, can be with it is an object of the present invention to provide a kind of manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy based on this
Improve aluminium neodymium alloy purity, reduce impurity content.
The purpose of the present invention is achieved through the following technical solutions:A kind of manufacture of magnetic controlled sputtering target timber-used aluminium neodymium alloy
Method, comprise the following steps:
S1:Aluminum feedstock and neodymium raw material are loaded in smelting furnace, carry out heating fusing, refining, casting, is made among aluminium neodymium and closes
Gold;
S2:Aluminium neodymium intermediate alloy obtained by step S1 is added in aluminum feedstock, loaded in smelting furnace, carry out heating fusing,
Refining, casting, are made aluminium neodymium alloy.
Relative to prior art, in two steps, the first step first prepares aluminium neodymium to manufacture method of the invention using aluminium and neodymium as raw material
Intermediate alloy, second step prepare aluminium neodymium alloy using aluminium and aluminium neodymium intermediate alloy as raw material again, due to aluminium neodymium intermediate alloy fusing point is low,
Proportion is low, purity is high, is more matched with the physicochemical property of aluminium, therefore there is preferably cooperation collaboration to make in fusion process for both
With, fusing time can be shortened, the problems such as overcoming splashing and be segregated, reduction pollution, and improve aluminium neodymium alloy purity, reduce impurity
Content, 99.999% can be reached by aluminium neodymium alloy purity produced by the present invention, so as to which aluminium neodymium alloy quality gets a promotion.
Further, the weight ratio of the aluminium component of the aluminium neodymium intermediate alloy and neodymium composition is 65:35.Due to the fusing point of aluminium
Less than neodymium, so neodymium just starts slowly to melt after aluminium fusing, and because neodymium thermal conductivity factor is low, cause it is outer it is hot in cold, and neodymium ratio
It is more crisp, easily cause to splash and cast gate remaining problem.65:Under 35 aluminium neodymium weight ratio, after aluminium has melted, because of the increasing of aluminium liquid amount
More, molten bath pressure increase, fusing point of the neodymium in fusion process is substantially reduced, and spattering problem is addressed, and cast gate remaining also subtracts
It is few.
Further, the particle diameter of the neodymium raw material is less than 0.2mm.The particle diameter of neodymium is less than 0.2mm, can prevent
Due to the higher caused local coking problem of temperature in fusion process, make fusing more uniform.
Further, in step S1, during charging, first fill aluminum feedstock and refill neodymium raw material.The aluminum feedstock of low melting point is first filled, is refilled
Dystectic neodymium raw material, lower tight upper pine, prevents from building bridge, fusion process is carried out in order.
Further, before charging, first the burner hearth in smelting furnace, crucible is cleared up, crucible is then preheated to 300
~400 DEG C.The cleanliness factor that can be improved in smelting furnace is cleared up burner hearth, crucible, reduces pollution;Crucible is preheated to
300~400 DEG C can prevent crucible stress under anxious heat condition is excessive to cause to ftracture.
Further, the vacuum in smelting furnace is 0.1~0.2Pa.Melting under vacuum, be advantageous to remove foreign gas,
The impurity that raw material is brought into simultaneously can volatilize under vacuum conditions, be purified material.
Further, in step S2, the weight ratio of aluminium neodymium intermediate alloy and aluminum feedstock is 5~80:100.The composition range
Interior aluminium neodymium intermediate alloy is added on aluminum substrate, can reduce material fusing point, shortens fusing time, and obtained aluminium neodymium alloy
Purity is high.
In order to more fully understand and implement, the present invention is described in detail with reference to specific embodiment.
Embodiment
Embodiment 1
The present embodiment provides a kind of manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy, comprises the following steps:
(1) aluminium neodymium intermediate alloy is prepared:Rafifinal of the purity more than 99% and high-purity neodymium are chosen as raw material, according to certain
Weight ratio carry out weighing dispensing, always feed intake 44kg;Before charging, first the burner hearth in smelting furnace, crucible are cleaned out, and by earthenware
Crucible is preheated to 300 DEG C;Aluminium is loaded in crucible, vacuumized, power per liter, after aluminium fusing, is slowly added into diameter less than 0.2mm's
Neodymium particle, after neodymium fusing, 35min is incubated at 1000 DEG C, vacuum is maintained at 0.1-0.2Pa, and frequency is maintained at 2000Hz;
After the completion of fusing, the molten metal after stirring fusing, it is sufficiently mixed alloy, and degasification, slagging-off, after liquid level purification, it is cooled to
900 DEG C, stand 20min;After the completion of purification, continue high-power stirring 3 times, then cast;After the completion of casting, 5min vacuum breakers,
Come out of the stove to obtain aluminium neodymium intermediate alloy.
(2) aluminium neodymium alloy is prepared:Aluminium neodymium intermediate alloy obtained by choosing rafifinal of the purity more than 99% and step (1) is made
For raw material, the weight ratio of aluminium neodymium intermediate alloy and aluminum feedstock is 5~80:100;Before charging, first by the burner hearth in smelting furnace, crucible
Clean out, and crucible is preheated to 300 DEG C;Aluminium is loaded in crucible, vacuumized, power per liter, after aluminium fusing, adds aluminium neodymium
Intermediate alloy, after the fusing of aluminium neodymium intermediate alloy, 35min is incubated at 1000 DEG C, vacuum is maintained at 0.1-0.2Pa, frequency
It is maintained at 2000Hz;After the completion of fusing, the molten metal after stirring fusing, it is sufficiently mixed alloy, and degasification, slagging-off, treat liquid level
After purification, 900 DEG C are cooled to, stands 20min;After the completion of purification, continue high-power stirring 3 times, then cast;Casting is completed
Afterwards, 5min vacuum breakers, come out of the stove to obtain aluminium neodymium alloy.
It is respectively 50 according to aluminium neodymium weight ratio in the preparation process of the aluminium neodymium intermediate alloy of the present embodiment step (1):50
(it is abbreviated as 50:50wt%), 60:40 (are abbreviated as 60:40wt%), 65:35 (are abbreviated as 65:35wt%) dispensing, tested
Aluminium neodymium intermediate alloy is prepared, it is as a result as follows:
Test for the first time:Prepare 50:50wt% aluminium neodymium intermediate alloys, in fusion process, because the fusing point of aluminium is 660
DEG C, thermal conductivity factor 0.53, the fusing point of neodymium is 1024 DEG C, thermal conductivity factor 0.031, so, after calorize is complete, neodymium just starts slowly
Fusing, because neodymium thermal conductivity factor is low, cause it is outer heat in it is cold, because neodymium is more crisp, cause splash it is very severe, pollution it is very serious, in addition
50:50wt% aluminium neodymium alloys fusing point is 1205 DEG C, causes cast gate remaining a lot, is not easy to feeding.Therefore, effect is undesirable.
Second of experiment:Prepare 60:40wt% aluminium neodymium intermediate alloys, tested compared to first time, reduce the content of neodymium,
But still can not be solved in fusion process, the problem of splashing, 60:40wt% aluminium neodymium alloys fusing point is 1020 DEG C, and cast gate is residual
It is a shade better compared with first time result of the test to send one's regards to topic, but it is undesirable.
Third time is tested:Prepare 65:35wt% aluminium neodymium intermediate alloys, compared to being tested for the first time with second, further
Reduce the content of neodymium, after calorize is complete, because of increasing for aluminium liquid amount, the increase of molten bath pressure, neodymium is in fusion process, spattering problem
It is addressed, has prevented pollution, meanwhile, 65:35wt% aluminium neodymium alloy fusing points are reduced to 820 DEG C, cast gate remaining greatly reduce to
Below 0.5kg, whole process is ideal, and intermediate alloy quality is very high.
Relative to prior art, in two steps, the first step first prepares aluminium neodymium to manufacture method of the invention using aluminium and neodymium as raw material
Intermediate alloy, second step prepare aluminium neodymium alloy using aluminium and aluminium neodymium intermediate alloy as raw material again, due to aluminium neodymium intermediate alloy fusing point is low,
Proportion is low, purity is high, is more matched with the physicochemical property of aluminium, therefore there is preferably cooperation collaboration to make in fusion process for both
With, fusing time can be shortened, the problems such as overcoming splashing and be segregated, reduction pollution, and improve aluminium neodymium alloy purity, reduce impurity
Content, 99.999% can be reached by aluminium neodymium alloy purity produced by the present invention, so as to which aluminium neodymium alloy quality gets a promotion.
Embodiment described above only expresses one embodiment of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.
Claims (7)
- A kind of 1. manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy, it is characterised in that:Comprise the following steps:S1:Aluminum feedstock and neodymium raw material are loaded in smelting furnace, carry out heating fusing, refining, casting, aluminium neodymium intermediate alloy is made;S2:Aluminium neodymium intermediate alloy obtained by step S1 is added in aluminum feedstock, loaded in smelting furnace, carry out heating fusing, refining, Casting, aluminium neodymium alloy is made.
- 2. the manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy according to claim 1, it is characterised in that:The aluminium neodymium The aluminium component of intermediate alloy and the weight ratio of neodymium composition are 65:35.
- 3. the manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy according to claim 2, it is characterised in that:The neodymium is former The particle diameter of material is less than 0.2mm.
- 4. the manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy according to claim 1, it is characterised in that:Step S1 In, during charging, first fill aluminum feedstock and refill neodymium raw material.
- 5. the manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy according to claim 1, it is characterised in that:Feed it Before, first the burner hearth in smelting furnace, crucible are cleared up, crucible is then preheated to 300~400 DEG C.
- 6. the manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy according to claim 1, it is characterised in that:In smelting furnace Vacuum be 0.1~0.2Pa.
- 7. the manufacture method of magnetic controlled sputtering target timber-used aluminium neodymium alloy according to claim 1, it is characterised in that:Step S2 In, the weight ratio of aluminium neodymium intermediate alloy and aluminum feedstock is 5~80:100.
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Cited By (1)
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CN114959595A (en) * | 2021-12-17 | 2022-08-30 | 常州苏晶电子材料有限公司 | High-purity aluminum-neodymium alloy target material for sputtering and manufacturing method thereof |
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