CN106637100A - Rare-earth metal target material and preparation method thereof - Google Patents
Rare-earth metal target material and preparation method thereof Download PDFInfo
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- CN106637100A CN106637100A CN201510729783.1A CN201510729783A CN106637100A CN 106637100 A CN106637100 A CN 106637100A CN 201510729783 A CN201510729783 A CN 201510729783A CN 106637100 A CN106637100 A CN 106637100A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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Abstract
The invention provides a rare-earth metal target material and a preparation method thereof. The preparation method comprises the following steps: step S1. smelting rare-earth metals into a rare-earth metal melt through a suspension smelting method adopting a water-cooled crucible; step S2. carrying out downward-drawing ingot casting on the rare-earth metal melt to obtain a rare-earth metal cast ingot; and step S3. carrying out forging rolling and machining on the rare-earth metal cast ingot to obtain the rare-earth metal target material. The melt can be prevented from being polluted by the crucible through using the suspension smelting method adopting the water-cooled crucible for smelting and carrying out the ingot casting in a downward-drawing manner, a relatively level solidification interface is obtained by virtue of the advantages that solidification shrinkage is compensated during a downward-drawing process to eliminate air vents and looseness, grain coarsening due to the rapid growth of dendritic crystals is avoided, and then the interior is enabled to be compact and defect-free; and therefore, the subsequent forging rolling is benefited, and the rare-earth metal target material with a large size can be obtained.
Description
Technical field
The present invention relates to target preparation field, in particular to a kind of rare earth metal target and preparation method thereof.
Background technology
IC industry technology follows Moore's Law and constantly develops evolution, wherein, chip constantly reduces its characteristic size, from micro-
Rice pushes deep-submicron to, and then marches toward nanometer era, and marches to the physics limit of microfabrication.As 28nm nodes of new generation
And following MOSFET (Metal-Oxide-Semiconductor Field-Effect Transistor, metal oxide semiconductcor field effect
Answer transistor) in gate insulating film require filming, but the SiO for using as gate insulating film so far2, because tunnel-effect is drawn
Play leakage current increase, it is difficult to normal operating.Accordingly, as its substitute, industry proposes steady with high-k, hyperpyrexia
It is qualitative and there is the HfO of high energy potential barrier to the hole in silicon and electronics2、ZrO2、Al2O3Non- rare earth metal oxide and
La2O3、Er2O3、Gd2O3、Yb2O3And Er2O3Deng rare earth oxide.Rare earth oxide in these materials is had higher rating,
It is expected to be replaced SiO2The electronic materials such as gate dielectric material, the metal gate material as high-k in MOSFET of new generation.
As sputtering Oxide rare earth thin film material rare earth metal target, no matter the aspect such as chemical purity or size be respectively provided with compared with
High request：Target purity is less than 100ppm more than 99.99wt%, O content；Target is little with diameter greater than 200mm, crystallite dimension
In 200 μm, and microstructure no significant defect etc..Especially for the fields such as semiconductor, display device rare earth metal target,
It requires purity, consistency, crystallite dimension, geometry and size etc. more strict.Especially in terms of purity, only make
The content of target rare earth element is not met by requirement more than 99.99wt%, and, calculating target rare earth metal in prior art
During content in rare earth metal target, typically the weight of target rare earth element deducts non-targeted rare earth with rare earth metal target material
The ratio of the weight difference after element wt, such denominator diminishes, and the purity for obtaining is naturally high.And in fact, other non-mesh
The presence of mark rare earth element can cause content of the target thulium in rare earth metal sheet material to be possible to not reach and be more than
The requirement of 99.99wt%.It is easily caused that film forming is uneven and film forming efficiency is low when such rare earth metal sheet material is used for into spatter film forming
Etc. defect.Thus, in addition it is also necessary to content of the target rare earth element in rare earth metal target is further improved, target is especially improved
Content ratio of the rare earth element relative to non-targeted rare earth element.
But because 99.99wt% purity rare earth metal product technologies of preparing realize that break through is still short in China, existing rare earth metal target
With 2N levels, (2N, 3N, 4N or 5N represent the purity of equivalent reagent to material preparation technology, and 4N refers to that content is 99.99%, N
Essence represent 9 number) commercially pure metal be raw material, using simple melting cast, then be cut to conform to requirement section bar,
The product of acquisition is mainly used in the traditional fields such as metallurgy.The characteristics of the method has process is simple, low cost, but product presence
Pore, crystallite dimension be larger, it is easy to crack the shortcomings of, it is difficult to meet the preparation requirement of large scale, high dense target material, and target
It is difficult to control the introducing of impurity in preparation process.In addition, comparatively, 4N levels metal is in intensity, hardness, plasticity, recrystallization
There is notable difference in the physical features such as temperature, existing rare earth target preparation technology has not been suitable for electronics with 2N technical pures metal phase ratio
The preparation of information target.
Thus, although also having the report of rare earth metal target more than a small amount of 4N levels in prior art, but these rare earth metals
Target is used to being easily caused when sputtering that film forming to be uneven and the low defect of film forming efficiency.Therefore, it is still necessary to which prior art is carried out
Improve, to provide a kind of high-purity rare earth metal target towards electronic information material and preparation method thereof.
The content of the invention
Present invention is primarily targeted at a kind of rare earth metal target and preparation method thereof is provided, to solve preparation of the prior art
Technique is difficult to meet problem prepared by the rare earth metal target of electronic information material.
To achieve these goals, according to an aspect of the invention, there is provided a kind of preparation method of rare earth metal target, is somebody's turn to do
Preparation method includes：Step S1, using cold-crucible suspension smelting method by rare earth metal metallurgy into rare earth metal liquation；Step
S2, to rare earth metal liquation drop-down ingot casting is carried out, and obtains rare earth metal ingot casting；And step S3, rare earth metal ingot casting is carried out
Forging rolling and machining, obtain rare earth metal target.
Further, rare earth metal is purity>The rare earth metal of 99.99wt%, preferred rare earth metal selected from La, Ce, Pr, Nd,
Any one in Gd, Tb, Dy, Ho, Er, Yb, Y and Sc.
Further, step S1 is implemented using suspension smelting furnace, the pressure superatmospheric 300～500Pa of power in suspension smelting furnace；
It is preferred that being argon gas atmosphere in suspension smelting furnace.
Further, step S2 carries out ultrasonically treated during drop-down ingot casting is carried out to rare earth metal liquation；Ultrasonically treated
The frequency range of ultrasonic wave is 30～40kHz in step, and the power of Ultrasound Instrument is less than or equal to 30kW.
Further, speed drop-down in step S2 is 0.5～1mm/min.
Further, step S3 includes：Step S31, by rare earth metal ingot casting predetermined temperature is heated to, and at a predetermined temperature
Open die forging is carried out successively in X-axis and Y direction to rare earth metal ingot casting, open die forging product is obtained；Step S32, to freedom
Forging product carries out cold rolling, obtains cold rolling product；And step S33, cold rolling product is heat-treated and is machined, obtain
Rare earth metal target.
Further, in step S31, predetermined temperature is 250～550 DEG C；Preferably, when rare earth metal is La, Ce or Yb
When, predetermined temperature is 250～310 DEG C；When rare earth metal is Nd or Pr, predetermined temperature is 300～400 DEG C；When rare earth gold
Belong to for Gd, Tb, Dy, Ho or Er when, predetermined temperature be 350～450 DEG C；When rare earth metal is Y or Sc, pre- constant temperature
Spend for 400～550 DEG C.
Further, in step S31, each open die forging causes the deflection of rare earth metal ingot casting to be more than 20%.
Further, in step S32, every time cold rolling deflection is more than 15%.
Further, heat treatment is carried out by the way of being tempered afterwards using first quenching under inert atmosphere protection, and quenching adopts the side of oil cooling
Formula is carried out, and the temperature of preferred quenching is 450 DEG C～650 DEG C, and the temperature of tempering is 150 DEG C～300 DEG C, and the time of tempering is 1～5h；
Preferably, the temperature of La, Ce or Yb quenching is 450 DEG C～550 DEG C, and the temperature of Nd or Pr quenchings is 500～600 DEG C, Gd,
The temperature of Tb, Dy, Ho or Er quenching is 550 DEG C～650 DEG C, and the temperature of Y, Sc quenching is 600～750 DEG C；Preferably,
La, Ce or Yb tempering temperature be 150 DEG C～200 DEG C, Nd or Pr tempering temperature be 200～250 DEG C, Gd, Tb, Dy,
The temperature of Ho or Er tempering is 200 DEG C～300 DEG C, and the temperature of Y, Sc tempering is 300～350 DEG C.
To achieve these goals, according to an aspect of the invention, there is provided a kind of rare earth metal target, the rare earth metal target
Material includes rare earth metal and impurity；Rare earth metal includes target rare earth metal and impurity rare earth metal, and target rare earth metal is in rare earth
Content in metal targets>99.99wt%, and content of the target rare earth metal in rare earth metal>99.999wt%, rare earth metal target
Oxygen content is less than 100ppm in material, and target rare earth metal is La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er, Yb, Y
And any one in Sc.
Further, the diameter of rare earth metal target>200mm；It is preferred that the average crystal grain particle diameter of rare earth metal target<200μm.
According to a further aspect in the invention, there is provided a kind of rare earth metal target, the rare earth metal target is using any of the above-described kind of system
Preparation Method is prepared from.
Using technical scheme, by carrying out melting, Neng Gouli to rare earth metal using cold-crucible suspension smelting method
Electromagnetic force is formed with alternating magnetic field, offseting with gravity makes melt suspend, and then disengages with crucible internal walls, is prevented from melting
Liquid is polluted by crucible, accordingly ensure that the rare earth metal liquation middle rare earth metal purity of institute's melting is higher.Then cast using pull-down pattern
Ingot, can compensate to solidification shrinkage, eliminate pore and it is loose wait coagulation defect, the opposed flattened freezing interface of generation is kept away
Exempt from dendrite and mushroom out to cause coarse grains, beneficial to forming the flawless smooth interface of interior solid, and then rolled by follow-up forging
System, is obtained in that large scale (diameter>Rare earth metal target 200mm).
Specific embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can be mutually combined.
The present invention is described in detail below in conjunction with embodiment.
As background section is previously mentioned, when using rare earth metal as raw material, it is difficult to make using preparation technology in prior art
It is standby to obtain qualified target, in order to improve above-mentioned condition, in a kind of typical embodiment of the present invention, there is provided a kind of rare earth
The preparation method of metal targets, the preparation method includes：Step S1, is melted in rare earth metal using cold-crucible suspension smelting method
It is smelt rare earth metal liquation；Step S2, to rare earth metal liquation drop-down ingot casting is carried out, and obtains rare earth metal ingot casting；And step
S3, forging rolling is carried out to rare earth metal ingot casting, then carries out machining to obtain rare earth metal target.
In the preparation method of above-mentioned rare earth metal target, by carrying out melting to rare earth metal using cold-crucible suspension smelting method,
Electromagnetic force can be formed using alternating magnetic field, offseting with gravity makes melt suspend, and then disengages with crucible internal walls, can
Prevent liquation from being polluted by crucible, accordingly ensure that the rare earth metal liquation middle rare earth metal purity of institute's melting is higher.Then using drop-down
Mode ingot casting, can compensate to solidification shrinkage, eliminate pore and loose wait coagulation defect, opposed flattened solidification circle of generation
Face, it is to avoid dendrite is mushroomed out causes coarse grains, beneficial to forming the flawless smooth interface of interior solid, and then by follow-up
Forging rolling, is obtained in that large scale (diameter>Rare earth metal target 200mm).
In the preparation method of above-mentioned rare earth metal target, rare earth metal can be any one in 17 kinds of rare earth metals, and rare earth is golden
The purity of category can adopt existing 2N levels, the rare earth metal of 3N levels, or the rare earth metal of 4N levels.Using above-mentioned water
Cold crucible levitation melting method carries out above-mentioned 2N levels, the rare earth metal of 3N levels of melting, compared to existing technology in other meltings
Mode, because smelting metal is not contacted with crucible internal walls, makes the content of metal targets middle rare earth metal higher, higher excellent of purity
Gesture.In a kind of preferred embodiment of the invention, using cold-crucible suspension smelting method by purity>The rare earth metal of 99.99wt%
Be smelt rare earth metal liquation, preferred rare earth metal include La, Pr, Nd, Gd, Ce, Tb, Dy, Ho, Er, Yb, Y with
And any one in Sc.The rare earth metal of mentioned kind is compared other rare earth metals and easily obtained to be had more than 4N ranks
Purity, is more beneficial for obtaining the higher rare earth metal target of purity using the rare earth metal of any of the above-described kind of 4N level.
In the preparation method of above-mentioned rare earth metal target, using cold-crucible suspension smelting method by rare earth metal metallurgy into rare earth gold
In the step of category liquation, according to the difference of the cold-crucible smelting in suspension equipment for specifically being used, concrete operations are suitably adjusted
.In a kind of preferred embodiment, rare earth metal metallurgy is being melted into rare earth metal using cold-crucible suspension smelting method
The step of liquid, implemented using suspension smelting furnace, wherein, the pressure superatmospheric 300～500Pa of power in suspension smelting furnace；
It is preferred that being argon gas atmosphere in suspension smelting furnace.
In above-mentioned preferred embodiment, in fusion process by the way of pressure-fired, i.e., the pressure in smelting furnace is slightly above air
The mode of 300～500Pa of pressure, under atmosphere of the inert gas such as argon gas, can effectively remove the higher metal impurities of vapour pressure
With the gaseous impurity such as O, N, H, it is ensured that rare earth metal is not only contaminated in fusion process, can further be purified on the contrary,
So that gaseous impurity content is in below 100ppm.
In the preparation method of above-mentioned rare earth metal target, can realize that fine and close smooth inside is flawless by the way of drop-down ingot casting
Rare earth metal ingot casting, in order to further improve the consistency and uniform ground degree of rare earth metal ingot casting, of the invention another kind of preferred
Embodiment in, in the step of carrying out drop-down ingot casting to above-mentioned rare earth metal liquation, obtain rare earth metal ingot casting, also include：
Ultrasonically treated step is carried out during drop-down ingot casting is carried out to rare earth metal liquation；Ultrasonic wave in ultrasonically treated step
Frequency range is 30～40kHz, and the power of ultrasonic wave is less than or equal to 30kW.
In above preferred embodiment, by during drop-down ingot casting, being oriented to rare earth metal liquation with reference to ultrasonic wave solidifying
Gu.The ingot casting in the way of continuous drop-down traction, can produce opposed flattened freezing interface, it is to avoid dendritic growth causes coarse grains,
And glass tube down-drawing can be compensated to solidification shrinkage, the coagulation defect such as pore and shrinkage cavity is eliminated；Apply ultrasonic wave in process of setting
Process, can crystal grain thinning, and increase homogenous nucleation rate, play a part of crystal grain thinning.With the method phase of traditional casting ingot-forming
Can obtain that high densification, high-purity, crystal grain is tiny, inside ingot no significant defect (gas than, the method in above preferred embodiment
Hole, crackle etc.) rare earth ingot casting, fully meet the requirement of follow-up large-size target processing.
In above preferred embodiment, the frequency range of ultrasonic wave is controlled in the range of 30～40kHz, and the power control of Ultrasound Instrument
System reduces the gas of inside ingot less than or equal in the range of 30kW, making thicker crystal grain be uniformly broken into small grains
The defect such as hole or crackle.But supersonic frequency is more than 30kW more than 40kHz, power, and grain refining effect is in the drop-down solidifying of the present invention
Gu under the conditions of weaken on the contrary, cause ingot casting hardness increase, it is difficult to forged；Frequency is more than 30kW less than 30kHz, power,
Thinning effect is not obvious, and is more likely formed micro- pore in inside ingot.
In carrying out the step of drop-down ingot casting obtains rare earth metal ingot casting to above-mentioned rare earth metal liquation, during drop-down ingot casting
Drop-down speed has no particular/special requirement, as long as rare earth metal liquation gradually cooling solidification in downdraw process can be made, is formed relatively flat
Whole freezing interface.In a kind of preferred embodiment of the invention, drop-down speed is during above-mentioned drop-down ingot casting
0.5～1mm/min.Ingot casting efficiency faster can be kept under the drop-down speed, and cooled and solidified interface can be caused opposed flattened,
And internal zero defect.
In above-mentioned preparation method, forging rolling is carried out to rare earth metal ingot casting, machining acquisition rare earth metal target is carried out again
The step of, can be according to the different of the requirement of concrete rare earth metal species and the rare earth metal target to be prepared by existing
Forging milling step carry out appropriate adjustment and obtain, as long as the rare earth metal target for meeting use requirement can be prepared.
In a kind of preferred embodiment of the invention, the step of forging rolling obtains rare earth metal target is carried out to rare earth metal ingot casting to be included：
Rare earth metal ingot casting is heated into predetermined temperature, and carries out in X-axis and Y direction open die forging successively under the predetermined temperature,
Obtain open die forging product；Open die forging product is carried out cold rolling, obtain cold rolling product；Cold rolling product is heat-treated, then is carried out
Machining obtains rare earth metal target.
In above preferred embodiment, by first heating to rare earth metal ingot casting, reach and carry out again after predetermined temperature open die forging,
Not only beneficial to the forging and molding of rare earth metal, and be conducive to improving the precision and quality of forging, then carry out open die forging, freely
The broken coarse grain of forging, and by heat treatment and the combination of free forging process, can crystal grain thinning, obtain the tiny (chi of crystal grain
It is very little<200 μm), the uniform microstructure of grain size also can remove machining stress, improve the lumber recovery of forging process.Then carry out
It is cold rolling, be conducive to obtaining the target blank dimension for meeting machining needs；Finally it is heat-treated, is conducive to removing cold working
Stress, forms recrystallization process and keeps material hardness.
In above-mentioned preparation method, in carrying out the step of heating reaches predetermined temperature to rare earth metal ingot casting, the predetermined temperature of heating
According to the different and different of concrete rare earth metal species, preferably 250～550 DEG C；It is highly preferred that when rare earth metal is La, Ce
Or during Yb, predetermined temperature is 250～310 DEG C；When rare earth metal is Nd or Pr, predetermined temperature is 300～400 DEG C；When
When rare earth metal is Gd, Tb, Dy, Ho or Er, predetermined temperature is 350～450 DEG C；When rare earth metal is Y or Sc,
Predetermined temperature is 400～550 DEG C.Predetermined temperature is arranged in above-mentioned different scope according to the different of rare earth metal species,
So that the inventive method adaptability is stronger so that above-mentioned various rare earth metals are in the case of identical active force, it is easier to deform,
Deflection enlarged relative, thus so that the deformation processing number of times of forging is relatively fewer.
In X-axis and Y direction open die forging is carried out successively after reaching a defined temperature in rare earth metal ingot casting, obtain open die forging product
The step of in, each open die forging cause the deflection of rare earth metal ingot casting according to the specific requirement of the metal targets to be prepared not
Different together, in a kind of specific embodiment of the invention, above-mentioned each open die forging causes the deflection of rare earth metal ingot casting to be more than
20%.Deformation amount controlling is in the range of more than 20% so that each deflection enlarged relative, in less deformation processing number of times
Can just reach the requirement of machining down, and with blank is high in machining efficiency, high yield rate benefit.
Similarly, it is above-mentioned open die forging product is carried out it is cold rolling obtain cold rolling product the step of in, every time cold rolling deflection is also
It is different according to the requirement of the target specifically to be prepared.The deflection cold rolling every time in another kind preferred embodiment of the invention
More than 15%.Deformation amount controlling cold rolling every time is had the advantage for improving finished product and heat treatment efficiency in the range of more than 15%.
Compare the target that acquisition is forged, rolled using conventional method, the rare earth metal utilized in above preferred embodiment it is pure
Degree reaches 4N levels, hardness less than industrial net product (HB, Brinell hardness is 30% 80), thus, using conventional heat treatment
Also rare earth metal target can be obtained, although section bar is not particularly suitable for sequent surface working process after rolling, it is difficult to ensure that target material surface is put down
Whole degree and fineness.In order to further improve follow-up processability, in another preferred embodiment of the invention, above-mentioned heat
Process is carried out under inert atmosphere protection using quenching and by the way of being tempered, and the temperature of quenching is 450 DEG C～650 DEG C, the temperature of tempering
Spend for 150 DEG C～300 DEG C, the time of tempering is 1～5h；Preferably, the temperature of La, Ce or Yb quenching is 450 DEG C～550 DEG C,
The temperature of Nd or Pr quenchings is 500～600 DEG C, and the temperature of Gd, Tb, Dy, Ho or Er quenching is 550 DEG C～650 DEG C；It is preferred that
Ground, La, Ce or Yb tempering temperature be 150 DEG C～200 DEG C, Nd or Pr tempering temperature be 200～250 DEG C, Gd, Tb,
The temperature of Dy, Ho or Er tempering is 200 DEG C～300 DEG C, and the temperature of Y or Sc tempering is 300～350 DEG C.
In above preferred embodiment, using the Technology for Heating Processing of quenching+tempering mode, maintain in the hardness for ensureing metal milling material
While Vickers hardness more than 70, the internal stress of quenching process generation is eliminated using tempering process, meet target material surface processing
Requirement to material plasticity and hardness, removes that macro morphology is uneven or " gnaw and cut " phenomenon from target, solves 4N level high-purity rare-earths
Target forms the problem of uneven film forming in sputter procedure because of rough surface.And for different rare earth metals, according to routine
The difference of hardness, plasticity and recrystallization temperature, the temperature of the temperature of quenching and tempering is controlled within the above range, to have respectively
The beneficial effect of technique strong applicability.
In another kind of typical embodiment of the invention, there is provided a kind of rare earth metal target, the rare earth metal target includes dilute
Earth metal and impurity, rare earth metal includes target rare earth metal and impurity rare earth metal, and target rare earth metal is in rare earth metal target
In content>99.99wt%, and target rare earth element is with respect to the content of total amount of rare earth>99.999%, oxygen content in rare earth metal target
Less than 100ppm, target rare earth metal is in La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er, Yb, Y and Sc
Any one.The purity of above-mentioned rare earth metal target middle rare earth metal is higher.
In another kind preferred embodiment of the invention, the diameter of above-mentioned rare earth metal target>200mm；It is preferred that rare earth metal target
Average crystal grain particle diameter<200μm.Crystal grain in above-mentioned rare earth metal target is more tiny, and microstructure evenly, is prepared
The direct size of rare earth metal target is bigger, can more meet the market demand.
In another typical embodiment of the invention, there is provided a kind of rare earth metal target, the rare earth metal target is using upper
State any one preparation method to be prepared from.The rare earth metal target prepared using above-mentioned preparation method not only rare earth metal purity
Height, and with high-compactness, internal zero defect, surfacing advantage, and obtained target is with diameter greater than 200mm.
Below in conjunction with specific embodiments further illustrating beneficial effects of the present invention.
Embodiment 1
The block lanthanum that purity is 99.9902% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 300Pa in control suspension smelting furnace, until block lanthanum is smelted into lanthanoid metal liquation；
By the water jacketed copper crucible for filling lanthanum liquation with the velocity pull-down of 0.5mm/min, lanthanum liquation gradually cools down solidifying in downdraw process
Gu while, lanthanum liquation is carried out ultrasonically treated with crystal grain thinning, obtain lanthanum ingot casting；Wherein the frequency of ultrasonic wave is 30kHz, is surpassed
The power of sound instrument is 30kW；
Lanthanum ingot casting is placed at a temperature of 250～310 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 25%, and each open die forging of X-axis to make lanthanum ingot casting maintain 250～310 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, heated again equally makes lanthanum ingot casting maintain 250～310 DEG C afterwards, so circulation, obtain freedom
Forging product；
Open die forging product is carried out cold rolling, and keep every time cold rolling deflection to be 16%, obtain cold rolling product；
Above-mentioned cold rolling product is heat-treated, heat treatment is carried out by the way of being tempered afterwards using first quenching, and cold rolling product is warming up to
450 DEG C are immediately placed in afterwards in oil and carry out oil cooling, carry out after tempering 1h at being placed in 150 DEG C again after oil cooling, then are machined
Obtain lanthanum target.
Embodiment 2
The thread praseodymium that purity is 99.9914% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 500Pa in control suspension smelting furnace, until thread praseodymium is smelted into praseodymium liquation；
By the water jacketed copper crucible for filling praseodymium liquation with the velocity pull-down of 1mm/min, the praseodymium liquation gradually cooled and solidified in downdraw process
While, praseodymium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain praseodymium ingot casting；Wherein the frequency of ultrasonic wave is 40kHz,
The power of Ultrasound Instrument is 20kW；
Praseodymium ingot casting is placed at a temperature of 300～400 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 22%, and each open die forging of X-axis to make praseodymium ingot casting maintain 300～400 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, heated again equally makes spectrum ingot casting maintain 300～400 DEG C afterwards, so circulation, obtain freedom
Forging product；
Open die forging product is put to carry out cold rolling, and keeps every time cold rolling deflection to be 18%, obtains cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, after open die forging
Product be warming up to 500 DEG C and be immediately placed in afterwards in oil and carry out oil cooling, carry out at being placed in 200 DEG C again after oil cooling after tempering 1.5h,
Machining is carried out again obtains praseodymium target.
Embodiment 3
The block cerium that purity is 99.9901% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under helium atmosphere,
Pressure superatmospheric power 450Pa in control suspension smelting furnace, until block cerium is smelted into cerium liquation；
By the water jacketed copper crucible for filling cerium liquation with the velocity pull-down of 0.8mm/min, cerium liquation gradually cools down solidifying in downdraw process
Gu while, cerium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain cerium ingot casting；Wherein the frequency of ultrasonic wave is 30kHz,
The power of Ultrasound Instrument is 25kW；
Cerium ingot casting is placed at a temperature of 250～310 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 23%, and each open die forging of X-axis to make cerium ingot casting maintain 250～310 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes cerium ingot casting maintain 250～310 DEG C, so circulation, obtain open die forging product
Thing；
Open die forging product is put to carry out cold rolling, and keeps every time cold rolling deflection to be 19%, obtains cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by cold rolling product liter
Temperature is immediately placed in afterwards in oil to 550 DEG C and carries out oil cooling, carries out after tempering 5h at being placed in 200 DEG C again after oil cooling, then carries out machine
Tool processing obtains cerium target.
Embodiment 4
The little block neodymium that purity is 99.9936% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 400Pa in control suspension smelting furnace, until little block neodymium is smelted into neodymium liquation；
By the water jacketed copper crucible for filling neodymium liquation with the velocity pull-down of 0.6mm/min, neodymium liquation gradually cools down solidifying in downdraw process
Gu while, neodymium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain neodymium ingot casting；Wherein the frequency of ultrasonic wave is 30kHz,
The power of Ultrasound Instrument is 15kW；
Neodymium ingot casting is placed at a temperature of 300～400 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 25%, and each open die forging of X-axis to make neodymium ingot casting maintain 300～400 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes neodymium ingot casting maintain 300～400 DEG C, so circulation, obtain open die forging product
Thing；
Open die forging product is put to carry out cold rolling, and keeps every time cold rolling deflection to be 17%, obtains cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by cold rolling product liter
Temperature is immediately placed in afterwards in oil to 600 DEG C and carries out oil cooling, carries out after tempering 2.5h at being placed in 250 DEG C again after oil cooling, then carries out machine
Tool processing obtains neodymium target.
Embodiment 5
The thread gadolinium that purity is 99.9938% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 400Pa in control suspension smelting furnace, until thread gadolinium is smelted into gadolinium liquation；
By the water jacketed copper crucible for filling gadolinium liquation with the velocity pull-down of 0.7mm/min, gadolinium liquation gradually cools down solidifying in downdraw process
Gu while, gadolinium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain gadolinium ingot casting；Wherein the frequency of ultrasonic wave is 40kHz,
The power of Ultrasound Instrument is 25kW；
Gadolinium ingot casting is placed at a temperature of 350～450 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 22%, and each open die forging of X-axis to make gadolinium ingot casting maintain 350～450 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes gadolinium ingot casting maintain 350～450 DEG C, so circulation, obtain open die forging product
Thing；
Open die forging product is put to carry out cold rolling, and keeps every time cold rolling deflection to be 19%, obtains cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by cold rolling product liter
Temperature is immediately placed in afterwards in oil to 550 DEG C and carries out oil cooling, carries out after tempering 1.5h at being placed in 200 DEG C again after oil cooling, then carries out machine
Tool processing obtains gadolinium target.
Embodiment 6
The thread dysprosium that purity is 99.9950% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 500Pa in control suspension smelting furnace, until thread dysprosium is smelted into dysprosium liquation；
By the water jacketed copper crucible for filling dysprosium liquation with the velocity pull-down of 1mm/min, the dysprosium liquation gradually cooled and solidified in downdraw process
While, dysprosium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain dysprosium ingot casting；Wherein the frequency of ultrasonic wave is 40kHz,
The power of Ultrasound Instrument is 20kW；
Dysprosium ingot casting is placed at a temperature of 350～450 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 21%, and each open die forging of X-axis to make dysprosium ingot casting maintain 350～450 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes dysprosium ingot casting maintain 350～450 DEG C, so circulation, obtain final freedom
Forging product；
Open die forging product is put down to carry out cold rolling, and keeps every time cold rolling deflection to be 16%, obtains cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by cold rolling product liter
Temperature is immediately placed in afterwards in oil to 650 DEG C and carries out oil cooling, carries out after tempering 3.5h at being placed in 300 DEG C again after oil cooling, then carries out machine
Tool processing obtains dysprosium target.
Embodiment 7
The thread yttrium that purity is 99.9931% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 500Pa in control suspension smelting furnace, until thread yttrium is smelted into yttrium liquation；
By the water jacketed copper crucible for filling yttrium liquation with the velocity pull-down of 0.9mm/min, yttrium liquation gradually cools down solidifying in downdraw process
Gu while, yttrium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain yttrium ingot casting；Wherein the frequency of ultrasonic wave is 30kHz,
The power of Ultrasound Instrument is 25kW；
Yttrium ingot casting is placed at a temperature of 400～550 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 25%, and each open die forging of X-axis to make yttrium ingot casting maintain 400～550 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes yttrium ingot casting maintain 400～550 DEG C, so circulation, obtain final freedom
Forging product；
Open die forging product is put down to carry out cold rolling, and keeps every time cold rolling deflection to be 16%, obtains cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by cold rolling product liter
Temperature is immediately placed in afterwards in oil to 650 DEG C and carries out oil cooling, carries out after tempering 4h at being placed in 320 DEG C again after oil cooling, then carries out machine
Tool processing obtains yttrium target.
Embodiment 8
The thread gadolinium that purity is 99.9938% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 400Pa in control suspension smelting furnace, until thread gadolinium is smelted into gadolinium liquation；
By the water jacketed copper crucible for filling gadolinium liquation with the velocity pull-down of 0.7mm/min, gadolinium liquation gradually cools down solidifying in downdraw process
Gu while, gadolinium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain gadolinium ingot casting；Wherein the frequency of ultrasonic wave is 40kHz,
The power of Ultrasound Instrument is 25kW；
Gadolinium ingot casting is placed at a temperature of 350～450 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 22%, and each open die forging of X-axis to make gadolinium ingot casting maintain 350～450 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes gadolinium ingot casting maintain 350～450 DEG C, so circulation, obtain open die forging product
Thing；
Open die forging product is carried out cold rolling, and keep every time cold rolling deflection to be 19%, obtain cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, heat treatment carried out using annealing way, by cold rolling product be warming up to 750 DEG C,
After insulation 1.5h, after naturally cooling to room temperature, then carry out machining and obtain gadolinium target.
Embodiment 9
The thread gadolinium that purity is 99.9938% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 400Pa in control suspension smelting furnace, until little block gadolinium is smelted into gadolinium liquation；
By the water jacketed copper crucible for filling gadolinium liquation with the velocity pull-down of 0.7mm/min, gadolinium liquation gradually cools down solidifying in downdraw process
Gu while, gadolinium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain gadolinium ingot casting；Wherein the frequency of ultrasonic wave is 40kHz,
The power of Ultrasound Instrument is 25kW；
Carry out forging rolling in accordance with the following steps to gadolinium ingot casting, heating gadolinium ingot casting simultaneously maintains 560 DEG C, carry out in any direction upsetting,
Cold rolling, every time deflection is 20%, is incubated 3.5h at 560 DEG C afterwards, after naturally cooling to room temperature, then carries out being machined
To gadolinium target.
Embodiment 10
The thread gadolinium that purity is 99.9938% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 280Pa in control suspension smelting furnace, until little block gadolinium is smelted into gadolinium liquation；
By the water jacketed copper crucible for filling gadolinium liquation with the velocity pull-down of 1.1mm/min, gadolinium liquation gradually cools down solidifying in downdraw process
Gu while, gadolinium liquation is carried out it is ultrasonically treated with crystal grain thinning, so as to obtain gadolinium ingot casting；Wherein the frequency of ultrasonic wave is 45kHz,
The power of Ultrasound Instrument is 25kW；
Gadolinium ingot casting is placed at a temperature of 300～450 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 20%, and each open die forging of X-axis to make gadolinium ingot casting maintain 350～450 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes gadolinium ingot casting maintain 350～450 DEG C, so circulation, obtain open die forging product
Thing；
Open die forging product is carried out cold rolling, and keep every time cold rolling deflection to be 14%, obtain cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by each open die forging
Product afterwards is warming up to 540 DEG C and is immediately placed in afterwards in oil and carries out oil cooling, and tempering 0.5h is carried out at being placed in 180 DEG C again after oil cooling
Afterwards, then carry out machining and obtain gadolinium target.
Comparative example 1
The block lanthanum that purity is 99.9902% is carried out into melting using electron beam (EB) stove, vacuum is 6 × 10-3～7 × 10-2Pa,
Jing direct pouring shapings, along with the furnace cooling room temperature form lanthanum ingot.
Carry out in an atmosphere and at a temperature of 400 DEG C to ingot casting rubbing forging, 300 DEG C～500 DEG C upsettings, machined formation lanthanum target
Material.
Comparative example 2
The thread gadolinium that purity is 99.9938% is put into the water jacketed copper crucible of suspension smelting furnace, melting is carried out under an argon atmosphere,
Pressure superatmospheric power 400Pa in control suspension smelting furnace, until thread gadolinium is smelted into gadolinium liquation；
Water jacketed copper crucible will be filled to topple over, gadolinium solution is poured onto in ingot mould and is quickly cooled to ingot casting；
Gadolinium ingot casting is placed at a temperature of 350～450 DEG C, carries out open die forging respectively along its X-axis and Y direction successively, every time certainly
It is to carry out heating after 22%, and each open die forging of X-axis to make gadolinium ingot casting maintain 350～450 DEG C by the deflection forged, then
The open die forging of Y-axis is carried out, carrying out heating again afterwards makes gadolinium ingot casting maintain 350～450 DEG C, so circulation, obtain open die forging product
Thing；
Open die forging product is carried out cold rolling, and keep every time cold rolling deflection to be 19%, obtain cold rolling product；
Above-mentioned cold rolling product is heat-treated, wherein, be heat-treated is carried out by the way of quenching plus tempering, by cold rolling product liter
Temperature is immediately placed in afterwards in oil to 550 DEG C and carries out oil cooling, carries out after tempering 1.5h at being placed in 200 DEG C again after oil cooling, then carries out machine
Tool processing obtains gadolinium target.
Detection：
The purity of the rare earth metal target middle rare earth metal prepared by the various embodiments described above and comparative example is examined using ICP methods
Survey；And the ratio of the content of all rare earth metals is accounted for purpose rare earth metal detected；Using the method for static testing to above-mentioned
The hardness of the rare earth metal target prepared by each embodiment is detected；Using slide calliper rule to the rare earth gold prepared by the various embodiments described above
The diameter of category target is detected；And its average crystal grain particle diameter is detected using metallography microscope method.Concrete testing result is shown in
Table 1.
Table 1：
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：The above-mentioned reality of the present invention
Apply example 1～10 and compare comparative example 1 and 2, by cold-crucible suspension smelting method, not only solve crucible to the pollution of melt and
Erosion problem of the melt to crucible, the melting for high pure rare earth metals provides Reliable guarantee.Meanwhile, by electricity in fusion process
The stirring action of magnetic force, drop-down ingot casting and ultrasonic wave are oriented solidification to rare earth metal, realize smelting in suspension and directional solidification
The mutual supplement with each other's advantages of two kinds of removal of impurities modes, can effectively remove the gaseous impurities such as Ca, Mg, K, Zn etc. and O, N, H, it is ensured that rare earth
Metal is not only contaminated in fusion process, is further purified on the contrary, can reach below 100ppm.
The ingot casting in the way of continuous drop-down traction, can produce opposed flattened freezing interface, it is to avoid dendrite is mushroomed out causes crystal grain
It is thick, and glass tube down-drawing can compensate to solidification shrinkage, eliminate pore and the coagulation defect such as loose；Apply in process of setting
Ultrasonic wave, can Broken Crystal, increase homogenous nucleation rate, play a part of crystal grain thinning.With the method for traditional casting ingot-forming
Compare, the above embodiment of the present invention can obtain that high densification, high-purity, crystal grain is tiny, inside ingot no significant defect (pore,
Crackle etc.) rare earth ingot casting, fully meet the requirement of follow-up large-size target processing.
Specifically, can be seen that embodiment 1～10 from the effect data of above-described embodiment 1～10 and comparative example 1 and 2 not only to exist
It is higher than comparative example 1 and 2 in purity, and the diameter of prepared target can reach more than 200mm, and comparative example 1 and 2
The diameter of prepared target is both less than 200mm.From embodiment 1 and comparative example 1 as can be seen that adopting identical raw material, press
Target of the average crystal grain particle diameter of the preparation method according to the present invention and the target prepared by the preparation method of comparative example 1 much smaller than comparative example
The average crystal grain particle diameter of material, and hardness is also greater than the hardness of the target of comparative example 1.Can be seen that from embodiment 5 and comparative example 2
The purity of the target prepared by the preparation method of the smelting in suspension method in combination with drop-down ingot casting of the present invention compared with smelting in suspension method with it is existing
Casting method prepared by target purity it is high, average crystal grain particle diameter is little, and hardness is big, thus the size of the target that can be prepared
Also more than 200mm can be reached.
In above-described embodiment, embodiment 8 and 9 is compared, embodiment 1-7 and embodiment 10 adopt Quenching plus tempering process,
The internal stress of quenching process generation is eliminated using tempering process, 4N grade high-purity rare earth metals is maintained using quenching technical and is added
Work hardening effect, obtains target hardness number>HB70, meets requirement of the target material surface processing to material plasticity and hardness.
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, for those skilled in the art
For, the present invention can have various modifications and variations.All any modifications within the spirit and principles in the present invention, made, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (13)
1. a kind of preparation method of rare earth metal target, it is characterised in that the preparation method includes：
Step S1, using cold-crucible suspension smelting method by rare earth metal metallurgy into rare earth metal liquation；
Step S2, to the rare earth metal liquation drop-down ingot casting is carried out, and obtains rare earth metal ingot casting；And
Step S3, carries out forging rolling and machining to the rare earth metal ingot casting, obtains the rare earth metal target.
2. preparation method according to claim 1, it is characterised in that the rare earth metal is purity>The rare earth gold of 99.99wt%
Category, the preferably rare earth metal are selected from La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er, Yb, Y and Sc
In any one.
3. preparation method according to claim 1, it is characterised in that step S1 is implemented using suspension smelting furnace, described
Pressure superatmospheric 300～500Pa of power in suspension smelting furnace；It is preferred that being argon gas atmosphere in the suspension smelting furnace.
4. preparation method according to claim 1, it is characterised in that step S2 is being carried out to the rare earth metal liquation
Carry out during drop-down ingot casting ultrasonically treated；The frequency range of ultrasonic wave is 30～40kHz in the ultrasonically treated step,
The power of Ultrasound Instrument is less than or equal to 30kW.
5. preparation method according to any one of claim 1 to 4, it is characterised in that drop-down speed in step S2
For 0.5～1mm/min.
6. preparation method according to claim 1, it is characterised in that step S3 includes：
Step S31, by the rare earth metal ingot casting predetermined temperature is heated to, and to rare earth gold under the predetermined temperature
Category ingot casting carries out successively open die forging in X-axis and Y direction, obtains open die forging product；
Step S32, carries out cold rolling to the open die forging product, obtains cold rolling product；And
Step S33, is heat-treated and is machined to the cold rolling product, obtains the rare earth metal target.
7. preparation method according to claim 6, it is characterised in that in step S31, the predetermined temperature is
250～550 DEG C；Preferably,
When the rare earth metal is La, Ce or Yb, the predetermined temperature is 250～310 DEG C；
When the rare earth metal is Nd or Pr, the predetermined temperature is 300～400 DEG C；
When the rare earth metal is Gd, Tb, Dy, Ho or Er, the predetermined temperature is 350～450 DEG C；
When the rare earth metal is Y or Sc, the predetermined temperature is 400～550 DEG C.
8. preparation method according to claim 6, it is characterised in that in step S31, every time the open die forging cause institute
The deflection for stating rare earth metal ingot casting is more than 20%.
9. preparation method according to claim 6, it is characterised in that in step S32, the every time cold rolling deflection
More than 15%.
10. preparation method according to claim 6, it is characterised in that the heat treatment under inert atmosphere protection using first quenching
The mode being tempered afterwards is carried out, and the quenching is carried out by the way of oil cooling, and preferably the temperature of the quenching is 450 DEG C～650 DEG C,
The temperature of the tempering is 150 DEG C～300 DEG C, and the time of the tempering is 1～5h；
Preferably, the temperature of La, Ce or Yb quenching is 450 DEG C～550 DEG C, and the temperature of Nd or Pr quenchings is 500～600 DEG C,
The temperature of Gd, Tb, Dy, Ho or Er quenching is 550 DEG C～650 DEG C, and the temperature of Y or Sc quenchings is 600～750 DEG C；
Preferably, the temperature of La, Ce or Yb tempering is 150 DEG C～200 DEG C, and the temperature of Nd or Pr tempering is 200～250 DEG C,
The temperature of Gd, Tb, Dy, Ho or Er tempering is 200 DEG C～300 DEG C, and the temperature of Y or Sc tempering is 300～350 DEG C.
11. a kind of rare earth metal targets, it is characterised in that the rare earth metal target includes rare earth metal and impurity；The rare earth metal
Including target rare earth metal and impurity rare earth metal, the target rare earth metal containing in the rare earth metal target
Amount>99.99wt%, and content of the target rare earth metal in the rare earth metal>99.999wt%, the rare earth metal
Oxygen content is less than 100ppm in target；The target rare earth metal be La, Ce, Pr, Nd, Gd, Tb, Dy, Ho,
Any one in Er, Yb, Y and Sc.
12. rare earth metal targets according to claim 11, it is characterised in that the diameter of the rare earth metal target>200mm；
It is preferred that the average crystal grain particle diameter of the rare earth metal target<200μm.
Rare earth metal target described in 13. claims 11 or 12, it is characterised in that the rare earth metal target adopts claim 1
It is prepared to the preparation method any one of 10.
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| CN110000211A (en) * | 2018-01-05 | 2019-07-12 | 宁波江丰电子材料股份有限公司 | Target milling method |
| CN112442622A (en) * | 2019-08-31 | 2021-03-05 | 苏州东宸先瑞新材料科技有限公司 | Production process of metal ytterbium target material |
| CN112725675A (en) * | 2020-12-23 | 2021-04-30 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN113106407A (en) * | 2021-03-26 | 2021-07-13 | 福建省长汀金龙稀土有限公司 | Manufacturing device and method of rare earth metal and rare earth alloy rotary target material |
| CN113652526A (en) * | 2021-07-21 | 2021-11-16 | 先导薄膜材料有限公司 | Heat treatment quenching method for target material |
| CN113846298A (en) * | 2021-09-27 | 2021-12-28 | 宁波江丰热等静压技术有限公司 | Preparation method of terbium target blank |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110000211A (en) * | 2018-01-05 | 2019-07-12 | 宁波江丰电子材料股份有限公司 | Target milling method |
| CN112442622A (en) * | 2019-08-31 | 2021-03-05 | 苏州东宸先瑞新材料科技有限公司 | Production process of metal ytterbium target material |
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| CN113106407A (en) * | 2021-03-26 | 2021-07-13 | 福建省长汀金龙稀土有限公司 | Manufacturing device and method of rare earth metal and rare earth alloy rotary target material |
| CN113652526A (en) * | 2021-07-21 | 2021-11-16 | 先导薄膜材料有限公司 | Heat treatment quenching method for target material |
| CN113652526B (en) * | 2021-07-21 | 2023-02-17 | 先导薄膜材料有限公司 | Heat treatment quenching method for target material |
| CN113846298A (en) * | 2021-09-27 | 2021-12-28 | 宁波江丰热等静压技术有限公司 | Preparation method of terbium target blank |
| CN113846298B (en) * | 2021-09-27 | 2023-11-07 | 宁波江丰热等静压技术有限公司 | Preparation method of terbium target blank |
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