CN104342619B - The preparation method of molybdenum target material - Google Patents
The preparation method of molybdenum target material Download PDFInfo
- Publication number
- CN104342619B CN104342619B CN201310331636.XA CN201310331636A CN104342619B CN 104342619 B CN104342619 B CN 104342619B CN 201310331636 A CN201310331636 A CN 201310331636A CN 104342619 B CN104342619 B CN 104342619B
- Authority
- CN
- China
- Prior art keywords
- target material
- molybdenum
- molybdenum target
- material blank
- hot
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
- B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of preparation method of molybdenum target material, including：First pass through the densification that hot-pressing sintering technique realizes molybdenum powder, obtain the first molybdenum target material blank, the first further densification of molybdenum target material blank is done step-by-step by multistage hot rolling treatment technique again afterwards, so as to obtain molybdenum grain less than 50 μm, consistency is up to 99.94% molybdenum target material.The molybdenum target material obtained relative to the molybdenum target material that existing molybdenum target material preparation method is obtained, the present invention molybdenum crystallite size is smaller, grain size evenly, consistency is higher, with more preferable electric property and machining property, fully meets molybdenum target material sputtering and requires.
Description
Technical field
The present invention relates to field of semiconductor manufacture, more particularly to a kind of preparation method of molybdenum target material.
Background technology
Molybdenum is a kind of silvery white non-ferrous metal, hard and tough and tensile, 2617 DEG C of its fusing point, 4612 DEG C of boiling point.Molybdenum has good at normal temperatures
Good corrosion resistance and stability, and relatively low specific impedance, good electric conductivity and good hot expansibility.Thus, molybdenum
It is widely used in the industries such as aerospace industry, electronics industry, glass work and photovoltaic.
Liquid crystal display in electron trade（Referred to as, LCD）Manufacture field.Because molybdenum distribution is matched somebody with somebody compared to traditional chromium
Line, can more effectively reduce specific impedance and the membrane stress of distribution, therefore molybdenum then can effectively lift liquid crystal for the component of LCD
Display screen brightness, contrast, color simultaneously extend the life-span；And the liquid crystal flat-panel using molybdenum shows and the environmental-protecting performance of touch-screen is strong, body
Small, the low advantage of power consumption of product.
Molybdenum is applied to LCD manufactures field by sputter coating process to form thin film manner mostly now；And in sputtering shape
Into in molybdenum film technique, the molybdenum target material quality for being used is the key factor of the molybdenum film quality to be formed.
The molybdenum target material of early stage is obtained by fusion casting, however, the consistency for adopting this method the molybdenum target material to be formed is difficult
To control.To solve the above problems, molybdenum target material is processed by the method using powder metallurgy in industry, i.e., by producing molybdenum powder
End, shaping is implemented to molybdenum powder and is sintered, and is then made molybdenum target material.Molybdenum powder metallurgy method has machinery, the thing of uniqueness due to it
Rationality energy, makes the consistency of the molybdenum target material of manufacture be improved compared to fusion casting.
Above-mentioned molybdenum target material PM technique refers to the Chinese patent literature of Publication No. CN102392222A.
However, with liquid crystal display maximization demand for development, the area of target is also increasing, at present conventional strip
The size of shape molybdenum target material is up to 2300 × 200 × 20mm.So for the consistency of target, and the careful requirement of crystal grain is tight all the more
Lattice.And the consistency of the large scale molybdenum target material that molybdenum target material PM technique is obtained is low now, only 80~90%, internal gas
Kong Duo, it is impossible to meet sputtering and require, to obtain good molybdenum film；And easily there is blank cracking phenomena during rolling,
Greatly reduce the yield rate of molybdenum target material preparation.
The content of the invention
The problem that the present invention is solved is to use hot pressed sintering and hot rolling technology, coordinates specific process conditions to be obtained
Consistency is up to 99.94%, and crystal grain is tiny, the large scale semiconductor molybdenum titanium sputtering target of even structure.
To solve the above problems, the present invention provides a kind of preparation method of molybdenum target material, including：
Molybdenum powder is provided；
Densification is carried out to molybdenum powder using hot-pressing sintering technique, the first molybdenum target material blank is formed；
Hot rolling treatment is carried out to the first molybdenum target material blank, the second molybdenum target material blank is formed；
After hot rolling treatment, annealing is carried out to the second molybdenum target material blank and forms molybdenum target material.
Alternatively, molybdenum powder is included using hot-pressing sintering technique：
Molybdenum powder is placed in mould；
After the mould is put into hot-pressed sintering furnace, by the hot pressed sintering stove evacuation；
The hot pressed sintering furnace temperature to 1200~1500 DEG C is adjusted, pressure is more than 20MPa, and 2~5h of heat-insulation pressure keeping.
Alternatively, the hot-pressing sintering technique also includes to being passed through protective gas in the hot-pressed sintering furnace.
Alternatively, the protective gas includes：Ar, He or N2。
Alternatively, the hot rolling treatment process includes, by the first molybdenum target material blank heating to 1200~1500 DEG C, it
After carry out rolling process.
Alternatively, after the hot rolling treatment, the deformation quantity of first target is more than 80%.
Alternatively, the rolling process is rolled including the multistage.
Alternatively, the rolling process includes three phases rolling process, and step is as follows：
First stage rolling is carried out to the first molybdenum target material blank, the deformation quantity for making the first molybdenum target material blank is
40%~60%；
Second stage rolling is carried out to the first molybdenum target material blank after the first stage rolls, makes first molybdenum target material
The deformation quantity of blank is 40%~60%；
After second stage, phase III rolling is carried out to the first molybdenum target material blank after second stage is rolled, obtained
Second molybdenum target material blank.
Alternatively, the first stage, second stage and phase III rolling process include multistep rolling mill practice；
After each step rolling mill practice of first stage rolling, the deformation quantity of the first molybdenum target material blank for 13~
40%；
After each step rolling mill practice of second stage rolling, the type variable of the first molybdenum target material blank is 5.5
~12%：
After each step rolling mill practice of second stage rolling, the type variable of the first molybdenum target material blank is 12.5
~20%.
Alternatively, the temperature of annealing less than or equal to hot-pressing sintering technique temperature, the temperature of annealing less than etc.
The temperature of second target during hot rolling treatment.
Alternatively, the method for the annealing is：Regulation temperature is 800~1200 DEG C, the second molybdenum described in Heat preservation
2~5h of target blank.
The preparation method of molybdenum target material according to claim 1, alternatively, the purity of the molybdenum powder is more than or equal to
99.95%, specific surface area is more than or equal to 1.1m2/g。
Compared with prior art, the technical program has advantages below：
During molybdenum powder carries out hot pressed sintering, pressurized, heated is carried out simultaneously, and under this condition, molybdenum powder occurs knot
Crystalline substance softens, and then thermoplasticity deformation occurs so that molybdenum interparticle contact spreads, and flowing mass transfer occurs, is misplaced between molybdenum powder close
Degree is increased considerably, and thus causes that molybdenum is intergranular to be bonded and reset, and molybdenum particle is mutually drawn close, the space between molybdenum particle it is total
Volume is reduced rapidly, and the grain boundary area between particle gradually increases, and so as to realize that the first time between molybdenum powder is densified, is obtained
First molybdenum target material blank；
Then in the hot rolling treatment technique for carrying out, the first molybdenum target material blank is rolled under the recrystallization temperature more than molybdenum
System, the larger molybdenum crystal grain of one side is broken, and molybdenum crystal grain is further refined, while dynamic knot occurs in the first molybdenum target material blank
Brilliant phenomenon, promotes molybdenum intercrystalline to be bonded again and reset, and reduces the space in the first molybdenum target material blank, improves the first molybdenum target material
Consistency；And, during hot rolling treatment, after high-temperature heating, there is recrystallization softening and shows the first molybdenum target material blank in molybdenum crystal grain
As, the first molybdenum target material blank plasticity of raising, and then the deformability of the first molybdenum target material blank is enhanced, compressing the first molybdenum target material
Sotck thinkness, the second molybdenum target material blank area obtained after increase hot rolling treatment technique simultaneously, is prevented effectively from based on the outer of rolling
Power and cause the first cracking phenomenon of molybdenum target material blank.
Further, hot rolling treatment is divided into multiple stages, and each stage includes the different rolling step of multistep deformation quantity
It is rapid with realize the first molybdenum target material blank progressively suppress, deformation, so as to further strengthen the densification effect of the first molybdenum target material blank,
During such scheme can also effectively alleviate the operation of rolling simultaneously, in the stress that the first molybdenum target material blank is internally formed, to avoid first
The defect such as molybdenum target material blank is cracking.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of the molybdenum target material that the present invention is provided；
Fig. 2~7 are the schematic diagrames of each step of preparation method of the molybdenum target material of the embodiment of the present invention；
Fig. 8~9 are the molybdenum target material crystal grain uniformity testing method schematic diagrames of the acquisition of the embodiment of the present invention.
Specific embodiment
As described in background, the large scale molybdenum target material consistency that the preparation technology of existing molybdenum target material is obtained is relatively low, nothing
Method meets target as sputter requirement.It is This invention provides a kind of preparation method of molybdenum target material.The molybdenum target material provided using the present invention
Preparation method can prepare consistency and be up to 99.94%, the mean grain size of molybdenum target material is less than 50 μm, and grainiess is uniform
Large scale molybdenum target material.Fully meet requirement of the magnetron sputtering for large scale molybdenum target material.
Below in conjunction with the accompanying drawings, by specific embodiment, clear, complete description is carried out to technical scheme.
First, with reference to shown in Fig. 1, step S1 is performed, there is provided molybdenum powder.
In the present embodiment, use to molybdenum powder purity more than or equal to 99.95%, specific surface area is more than or equal to
1.1m2/g。
In follow-up hot pressed sintering, hot rolling treatment and annealing process, it is based on crystallization softening by molybdenum particle and sends out
In raw plastic history, the heat energy that the hot and outside that intergranular friction, shearing-crushing deform and produce is granted so that molybdenum is brilliant
The crystal boundary of intergranular melts, and in the process, the specific surface area of molybdenum powder is bigger, then crystal boundary fuses area more in compacting process
Greatly, so as to be favorably improved the target consistency to be formed.Originally it is that the specific surface area of the molybdenum powder of use is more than in embodiment
1.1m2/ g, can help to improve the target consistency being subsequently formed, and reduce the energy for promoting each intercrystalline to fuse in preparation process
Consumption.
Step S2 is performed, densification is carried out to the molybdenum powder 10 using hot-pressing sintering technique, form the first molybdenum target
Material blank.
Detailed process refers to Fig. 2 and Fig. 3, including：
Referring initially to Fig. 2, enough molybdenum powders 10 are placed in graphite jig 20, graphite jig 20 is positioned over into hot pressing afterwards burns
In freezing of a furnace 30, by the hot pressed sintering stove evacuation；Referring next to Fig. 3, adjust the regulation temperature of hot-pressed sintering furnace 30 to
1200~1500 DEG C, such as 1200 DEG C, 1250 DEG C, 1300 DEG C, 1350 DEG C, 1400 DEG C, 1450 DEG C and 1500 DEG C, regulation pressure to heat
Pressure in pressure sintering furnace 30 is more than 20MPa, 2~5h of heat-insulation pressure keeping, realizes the densification of the molybdenum powder 10, to obtain the
One molybdenum target material blank 11.
During hot pressed sintering, under high temperature, condition of high voltage, molybdenum powder 10 is activated the molybdenum powder 10, molybdenum powder
10 crystallization soften and there is thermoplasticity deformation, in hot plastic state molybdenum powder between contact diffusion, occur flowing mass transfer motion.And
Advance over time, dislocation density is increased considerably between molybdenum powder, molybdenum is intergranular to be bonded and reset, and is mutually leaned between particle
Hold together, and it is bonded mutually, and crystal grain is grown up, and the space between molybdenum particle is reduced rapidly, and crystal boundary is gradually reduced, and molybdenum particle overall volume is received
Contracting, the grain boundary area between particle gradually increases so that target blank density increases, it is achieved thereby that the densification between molybdenum powder
Change.
After above-mentioned hot-pressing sintering technique, the consistency of the first molybdenum target material blank 11 of acquisition can reach 93~98%, averagely
Molybdenum crystallite size is less than 100 μm.And the hot rolling treatment for after is prepared.
During hot pressed sintering, it is necessary to assure enough temperature to realize the crystallization softening and plastic deformation of particle, with true
Being bonded between protection granules and reset.But too high temperature can cause molybdenum grain crystalline excessive, so as to reduce the target blank of acquisition
Consistency.In the present embodiment, the hot pressed sintering temperature control is ensuring molybdenum powder particle at this temperature in 1200~1500 DEG C
Plastic deformation, and realize densification simultaneously, it is to avoid temperature is too high and cause the excessive phenomenon of molybdenum grain crystalline.
It should be noted that can further improve the first molybdenum of acquisition by further strengthening the pressure of hot-pressing sintering technique
The consistency of target blank 11, but too high pressure not only needs to consume bigger energy consumption, can also further increase hot pressed sintering
For the requirement of equipment, if desired for the stronger grinding tool of crushing resistance, hot pressing is caused to avoid mould during hot pressed sintering impaired
Sintering process fails.In addition excessive pressure is imposed in hot-pressing sintering technique can also cause molybdenum target material blank cracking existing
As.
In the present embodiment, the pressure of the hot-pressing sintering technique more than 20MPa just can, such as 20MPa, 25MPa, 30MPa,
35MPa etc., the hot pressed sintering pressure compared to existing 60MPa or so in the present embodiment, is coordinated by above-mentioned hot-pressing sintering technique
While such as hot rolling treatment technique subsequent technique finally obtains high-compactness molybdenum target material, also effectively reduction molybdenum target material work can be prepared
The energy consumption of skill, for such as equipment requirement such as graphite jig or hot-pressed sintering furnace.
In other examples, during hot-pressing sintering technique, can also be to being passed through such as in the hot-pressed sintering furnace
Ar, He or N2Deng protective gas, with the further impurity component reduced in the first molybdenum target material blank 11 for being formed, and hot pressing is ensured
Sintering process stability.
With continued reference to shown in Fig. 1, step S3 is performed, hot rolling treatment is carried out to the first molybdenum target material blank 11, so as to enter
One step is densified the structure of the first molybdenum target material blank 11, obtains the second molybdenum target material blank.In the present embodiment, specific steps can be tied
Close and refer to Fig. 4~Fig. 6：
Referring initially to shown in Fig. 4, in the present embodiment, the mode of the hot rolling is in calender by the second molybdenum target material blank 12
Extruded between two rollers 40a and 40b, so that by relative both direction simultaneously for the first molybdenum target material blank 11
Carry out single shaft extruding.The technical scheme can effectively improve the rolling efficiency of the first molybdenum target material blank 11 simultaneously, first molybdenum target
The deformation uniformity of each several part of the through-thickness of material blank 11, with the second molybdenum target material blank 12 for ensuring to be obtained after hot rolling treatment
The uniformity of grain structure.
The hot rolling treatment includes：The second molybdenum target material blank 12 is first carried out into pre-add heat treatment so that described second
The temperature of molybdenum target material blank 12 is 1200~1500 DEG C, and now, the temperature of the molybdenum target material blank 11 is more than recrystallization temperature, it
Carry out rolling process again afterwards.In the operation of rolling, larger molybdenum crystal grain is broken in the first molybdenum target material blank 11, molybdenum
Crystal grain is further refined, to reduce the space in the first molybdenum target material blank, and in the operation of rolling, the molybdenum target material blank
11 there is dynamic recrystallization phenomenon, and the molybdenum intercrystalline after simply crushing is bonded and resets again, so as to the first molybdenum can be effectively improved
The equal consistency of crystal grain in target blank.Additionally, in the operation of rolling, the temperature of the molybdenum target material blank 11 is more than recrystallization temperature
Degree so that the molybdenum particle recrystallization softening in the first molybdenum target material blank 11, in mecystasis, effectively improves described the
The plasticity of one molybdenum target material blank 11, and then reduce the ability of anti-deformation of the first molybdenum target material blank 11.At high operating temperatures first
In the operation of rolling of molybdenum target material blank 11, while compression the first molybdenum target material sotck thinkness increase target blank area, can also have
Effect prevents the cracking phenomenon of target blank.
Referring next to shown in Fig. 5, after the hot rolling treatment, the deformation quantity of the first molybdenum target material blank 11 is excellent more than 80%
Elect 80~90% as, i.e. the thickness of the first molybdenum target material blank 11 is h, the second molybdenum target material blank 12 obtained after hot rolling treatment
Thickness be H,（h-H）/ h=80~90%（As shown in Figure 5）.During hot rolling treatment, the first molybdenum target material blank 11
Thickness is compressed, and upper and lower surface product becomes big, so as to obtain large-sized second molybdenum target material blank 12.
In the operation of rolling, it is cracking that excessive deformation quantity likely results in target blank, in the present embodiment, to prevent
First molybdenum target material blank 11 ftractures, to preheating after the first molybdenum target material blank 11 the multiple stage rollings treatment of rolling process point.
And in different phase, can be by being such as stepped up imposing on the pressure of the first molybdenum target material blank 11, so as to realize that target is progressively rolled
Deformation.Wherein, the rolling process in each stage can be divided into multiple steps and carry out again.
Specifically, the rolling process includes three phases：
With reference to shown in reference to Fig. 6：
A, first stage rolling first is carried out to the first molybdenum target material blank 11, make to state the thickness of the first molybdenum target material blank 11
Degree deformation quantity is 40%~60%.
In the present embodiment, the thickness of the first molybdenum target material blank 11 is obtained after hot pressed sintering for 100~150mm, the first rank
After section rolling, the thickness of the first molybdenum target material blank of acquisition is 40~90mm.
Wherein, the rolling mill practice of the first stage divide again can for multistep is carried out, and each step rolling after, first molybdenum
The deformation quantity of target blank 11 is 13~40%, and in such as Fig. 6, the first molybdenum target material blank 11 before A step rollings is h1, and A steps are rolled
The first molybdenum target material blank 11 after system is h2,（h1-h2）/ h1=13~40%.
In the present embodiment, in the first stage in the operation of rolling, after being rolled through each step, the first molybdenum target material blank 11
Thickness reduces by 10~20mm.
B, the first molybdenum target material blank 11 obtained after being rolled through the first stage carry out second stage rolling so that described the
The thickness deformation quantity of one molybdenum target material blank 11 reaches 40%~60%.
In the present embodiment, after first stage rolling, the thickness of the first molybdenum target material blank of acquisition is 40~90mm,
After through the rolling of second stage, the thickness of the first molybdenum target material blank 11 is changed into 16mm~54mm.
Wherein, the rolling mill practice of the second stage equally divides and can be carried out for multistep, and after the rolling of each step, described first
The deformation quantity of molybdenum target material blank 11 is 5.5~12%.As in Fig. 6, the first molybdenum target material blank 11 before B step rollings is h1, B
The first molybdenum target material blank 11 after step rolling is h2,（h1-h2）/ h1=5.5~12%.
In the present embodiment, in the second stage operation of rolling, after being rolled through each step, the first molybdenum target material blank 11
Thickness reduces by 2~3mm
C, the first molybdenum target material blank 11 to being obtained through second stage rolling carry out phase III rolling, until rolling is final
The thickness of the molybdenum target material blank of needs, obtains the second molybdenum target material blank 12.
Wherein, the rolling mill practice of the phase III equally divides and can be carried out for multistep, and after the rolling of each step, described first
The deformation quantity of molybdenum target material blank 11 is 12.5~20%.As in Fig. 6, the first molybdenum target material blank 11 before B step rollings is h1, B
The first molybdenum target material blank 11 after step rolling is h2,（h1-h2）/ h1=12.5~20%.
In the present embodiment, in the phase III operation of rolling, after each step rolling, the thickness of the first molybdenum target material blank 11
Degree reduces 1mm or so.
As rolling is carried out in the above three stage, the consistency of the first molybdenum target material blank 11 of acquisition is constantly lifted.And
And coordinate the amount of the consistency of the first molybdenum target material blank 11 lifting, each stage substep rolling to be gradually reduced, so as to be prevented effectively from
In the operation of rolling, the cracking phenomenon of target blank, and then obtain high-compactness molybdenum target material simultaneously, lifting molybdenum target material prepare into
Product rate.
Thickness by after above-mentioned hot rolling treatment, effectively reducing the first molybdenum target material blank 11, increased target blank
Area.Meanwhile, after hot rolling treatment, further optimize the internal structure of molybdenum target material blank, in the present embodiment, acquisition it is described
Molybdenum crystallite size in second molybdenum target material blank 12 is less than 50 μm（Method of testing：GB T6394-2002, metal average crystal grain is surveyed
Determine method）, and consistency is up to 99.94%（Method of testing：GB3850-83 ≈ ISO3369-1975, dense sintering metal material
With hard alloy density measurement method）.
In the alternative of the hot rolling treatment of the present embodiment, after the preheating of the first molybdenum target material blank 11 is completed,
The first molybdenum target material blank 11 can be in H2Or such as Ar, He or N2Rolled under protection Deng inert gas.So as to have
Effect avoids the first molybdenum target material blank 11 described in the operation of rolling that serious oxidative phenomena occurs.
With continued reference to shown in Fig. 1, step S4 is performed, annealing is carried out to the second molybdenum target material blank 12 and forms molybdenum target
Material.
Specifically refer to shown in Fig. 7, in the present embodiment, the second molybdenum target material blank 12 is obtained through above-mentioned hot rolling treatment
Afterwards, the second molybdenum target material blank 12 is put into heating furnace 50 and is made annealing treatment, obtain molybdenum target material.
The annealing process includes：The second molybdenum target material blank 12 is heated to 800~1200 DEG C, and continue insulation plus
2~5h of heat.The temperature of the annealing and heat time make specific adjustment according to actual conditions, and the annealing temperature is less than it
Temperature in preceding hot pressed sintering and hot rolling treatment.
In above-mentioned annealing process, the interior tissue of the second molybdenum target material blank 12 is recrystallized to reach balance
State so that the crystal grain inside second copper target blank is changed into more uniform equi-axed crystal；In addition annealing can make
Before obtaining in hot rolling technology, the stress being formed in second copper target blank 12 is fully discharged so that target blank
Internal structure further optimized, improve the second copper target material mechanical performance and stability.
In the second molybdenum target material blank 12 in annealing process, if temperature is too low, the heat time is too short, the second molybdenum
The crystal grain of target blank 12 is heated uneven, it is impossible to the stress fully in the second molybdenum target material blank of release；But if temperature is too high, plus
Hot overlong time, the crystal grain of the second molybdenum target material blank 12 is easily grown up, and intercrystalline space becomes big, so as to influence the copper to be formed
The consistency of target.
In the present embodiment, the temperature of the annealing less than or equal to the temperature in above-mentioned hot-pressing sintering technique, and less than etc.
In above-mentioned hot forging processing procedure, the temperature of the first molybdenum target material blank 11.Specifically, the temperature in described annealing process
It it is 800~1200 DEG C, the time of annealing continues 2~5 hours.Through inspection, the molybdenum crystallite size in the molybdenum target material obtained after annealing
It still is below 50 μm（Method of testing：GB T6394-2002, metal average crystal grain assay method）, consistency still reaches 99.94%
（Method of testing：GB3850-83 ≈ ISO3369-1975, dense sintering metal material and hard alloy density measurement method）.This
Above-mentioned annealing process in embodiment, both can ensure that the stress in the second molybdenum target material blank 12 fully discharged, and can avoid what is obtained again
The reduction of molybdenum target material consistency.
After the annealing process, the molybdenum target material blank for obtaining is machined, the molybdenum target material 13 of size needed for being formed.
With reference to shown in Fig. 8, after molybdenum target material 13 is obtained, multiple sections are divided on wooden target 13（3 are shown as in figure each disconnected
Face）, and multiple sample points are obtained on cross sections, carry out the size test of molybdenum crystal grain.Fig. 9 is some test numbers of this implementation
According to curve.Fig. 9 is shown in the present embodiment, on the molybdenum target material for obtaining along a straight line on 3 sections being evenly dividing,
The grain size data on 10 sample points for obtaining at random respectively.
Shown according to data and curves, the grain size of the molybdenum target material obtained in the present embodiment in view of between 32~47 μm, most
Big span is no more than 15 μm.It follows that the present embodiment obtain molybdenum target material with the excellent crystal grain uniformity.
In the present embodiment, it is 1200~1500 DEG C to first pass through temperature, and pressure realizes molybdenum powder up to the hot-pressing sintering technique of 20MPa
The densification at end, to obtain molybdenum grain less than 100 μm, consistency is 93~98% the first molybdenum target material blank, afterwards
The first further densification of molybdenum target material blank is done step-by-step by multistage hot rolling treatment technique again, so as to obtain molybdenum
Grain crystal grain is less than 50 μm, and consistency is up to 99.94% molybdenum target material；And annealing process can be in further optimization target internal junction
On the basis of structure, the mechanical performance of target, and stability are improved.
Compared to the molybdenum target material that existing induction sintering technology and hot rolling technique are obtained, the molybdenum of the molybdenum target material that this implementation is obtained
Crystallite size is smaller, and evenly, consistency is higher for grain size, so that there is more preferable electric property and machining property,
Required so as to meet molybdenum target material sputtering.Additionally, in the present embodiment each procedure of processing mild condition, it is more easy to control, and effectively keep away
Exempt from process, the phenomenon of each stage target cracking effectively increases the yield rate of molybdenum target material preparation.
Although the present invention is disclosed as above with preferred embodiment, it is not for limiting the present invention, any this area
Technical staff without departing from the spirit and scope of the present invention, may be by the methods and techniques content of the disclosure above to this hair
Bright technical scheme makes possible variation and modification, therefore, every content without departing from technical solution of the present invention, according to the present invention
Any simple modification, equivalent variation and modification for being made to above example of technical spirit, belong to technical solution of the present invention
Protection domain.
Claims (6)
1. a kind of preparation method of molybdenum target material, it is characterised in that including：
Molybdenum powder is provided；
Densification is carried out to molybdenum powder using hot-pressing sintering technique, the first molybdenum target material blank is formed；
Hot rolling treatment is carried out to the first molybdenum target material blank, the second molybdenum target material blank is formed；
After hot rolling treatment, annealing is carried out to the second molybdenum target material blank and forms molybdenum target material；
The hot rolling treatment process includes, by the first molybdenum target material blank heating to 1200~1500 DEG C, is rolled afterwards
Treatment；
The rolling process includes three phases rolling process, and step is as follows：
First stage rolling is carried out to the first molybdenum target material blank, make the deformation quantity of the first molybdenum target material blank for 40%~
60%；
Second stage rolling is carried out to the first molybdenum target material blank after the first stage rolls, is made after the first stage rolls
The first molybdenum target material blank deformation quantity be 40%~60%；
After second stage, phase III rolling is carried out to the first molybdenum target material blank after second stage is rolled, obtain second
Molybdenum target material blank；
Molybdenum powder is included using hot-pressing sintering technique：
Molybdenum powder is placed in mould；
After the mould is put into hot-pressed sintering furnace, by the hot pressed sintering stove evacuation；
The hot pressed sintering furnace temperature to 1200~1500 DEG C is adjusted, pressure is more than 20MPa, and 2~5h of heat-insulation pressure keeping.
2. the preparation method of molybdenum target material according to claim 1, it is characterised in that the hot-pressing sintering technique also include to
Protective gas is passed through in the hot-pressed sintering furnace.
3. the preparation method of molybdenum target material according to claim 2, it is characterised in that the protective gas includes：Ar, He or
N2。
4. according to the preparation method of the molybdenum target material described in claim 1, it is characterised in that after the hot rolling treatment, first molybdenum
The deformation quantity of target blank is more than 80%.
5. the preparation method of molybdenum target material according to claim 1, it is characterised in that the method for the annealing is：Adjust
Section temperature is 800~1200 DEG C, second 2~5h of molybdenum target material blank described in Heat preservation.
6. the preparation method of molybdenum target material according to claim 1, it is characterised in that the purity of the molybdenum powder is more than or equal to
99.95%, specific surface area is more than or equal to 1.1m2/g。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310331636.XA CN104342619B (en) | 2013-07-31 | 2013-07-31 | The preparation method of molybdenum target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310331636.XA CN104342619B (en) | 2013-07-31 | 2013-07-31 | The preparation method of molybdenum target material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104342619A CN104342619A (en) | 2015-02-11 |
| CN104342619B true CN104342619B (en) | 2017-06-30 |
Family
ID=52499063
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310331636.XA Active CN104342619B (en) | 2013-07-31 | 2013-07-31 | The preparation method of molybdenum target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104342619B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105525260A (en) * | 2014-10-22 | 2016-04-27 | 宁波江丰电子材料股份有限公司 | Production methods of Mo target blank and Mo target material |
| CN105483626B (en) * | 2015-12-09 | 2018-01-16 | 西安瑞福莱钨钼有限公司 | A kind of production method of fine grain planar molybdenum target material |
| CN108950494A (en) * | 2018-07-30 | 2018-12-07 | 常州苏晶电子材料有限公司 | The production method of strip molybdenum target material |
| CN112091343A (en) * | 2020-09-11 | 2020-12-18 | 宁波江丰电子材料股份有限公司 | Brazing method of molybdenum target and back plate |
| CN112609162B (en) * | 2020-12-10 | 2023-04-04 | 宁波江丰钨钼材料有限公司 | LCD molybdenum target material and rolling method and application thereof |
| CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057000A (en) * | 2004-08-31 | 2007-10-17 | H.C.施塔克公司 | Molybdenum sputtering targets |
-
2013
- 2013-07-31 CN CN201310331636.XA patent/CN104342619B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057000A (en) * | 2004-08-31 | 2007-10-17 | H.C.施塔克公司 | Molybdenum sputtering targets |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104342619A (en) | 2015-02-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104342619B (en) | The preparation method of molybdenum target material | |
| CN104439247B (en) | The preparation method of molybdenum alloy target | |
| CN103071793B (en) | Molybdenum sputtering target material hot isostatic pressure production method | |
| CN102121078B (en) | Composite preparation method for fine crystal titanium alloy | |
| CN104846341A (en) | Isothermal extrusion production method of refractory metal rotating target material | |
| CN104419901B (en) | A kind of manufacture method of tantalum target | |
| CN108642457B (en) | Production method of high-generation molybdenum target | |
| CN102218535B (en) | Sintering method for molybdenum product | |
| CN103121848B (en) | A kind of aluminum nitride ceramic substrate sintering process | |
| CN106319457A (en) | Manufacturing method of tungsten titanium tube target | |
| CN103805952B (en) | A kind of large scale high purity tungsten target and production method thereof | |
| CN104057667B (en) | A kind of TiAl/Ti 3siC 2composite board and preparation method thereof | |
| CN110538993A (en) | preparation process of high-density molybdenum-tantalum alloy sputtering target material | |
| CN104773998A (en) | Sintering method of high-density ITO target | |
| CN104496473A (en) | Production method of high-density conductive niobium oxide target | |
| CN102699328B (en) | Process for manufacturing large molybdenum electrode | |
| CN106424741B (en) | SiC particulate enhances intermetallic compound base laminar composite Ti/Al3The preparation method of Ti | |
| CN103556094B (en) | Utilize the method for precise forging machine forging TC4 titanium alloy rod bar | |
| CN105568237A (en) | Chromium-molybdenum alloy target material preparation method | |
| CN106270530A (en) | A kind of manufacture method of high density pure rhenium test tube | |
| US9506141B2 (en) | Method for manufacturing a molybdenum sputtering target for back electrode of CIGS solar cell | |
| CN105543735A (en) | Method for eliminating beta/B2 phase in casting high-Nb-TiAl alloy | |
| CN104942291B (en) | A kind of hot-pressing sintering method of Ti 6Al 4V alloys | |
| CN106475567A (en) | The manufacture method of chrome molybdenum target blankss | |
| CN107761062B (en) | Method for manufacturing target blank and target assembly |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211101 Address after: 516001 room 1803t, 18th floor, innovation building, No. 106, Dongxin Avenue, Dongjiang Industrial Park, Zhongkai high tech Zone, Huizhou, Guangdong Patentee after: Guangdong Jiangfeng Electronic Material Co.,Ltd. Address before: 315400 Ningbo City, Zhejiang Province 198 Anshan Road, Mingbang science and Technology Industrial Park, Yuyao City, Zhejiang Province Patentee before: KONFOONG MATERIALS INTERNATIONAL Co.,Ltd. |
|
| TR01 | Transfer of patent right |