CN108640685A - A kind of preparation method of molybdenum disulfide target - Google Patents
A kind of preparation method of molybdenum disulfide target Download PDFInfo
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- CN108640685A CN108640685A CN201810795425.4A CN201810795425A CN108640685A CN 108640685 A CN108640685 A CN 108640685A CN 201810795425 A CN201810795425 A CN 201810795425A CN 108640685 A CN108640685 A CN 108640685A
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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Abstract
The invention discloses a kind of preparation methods of molybdenum disulfide target, include the following steps：The pretreatment of molybdenum disulfide powder, obtains mixed material；Isostatic pressing is carried out to mixed material and is pressed into blocky crude green body；Blocky crude green body is put into atmosphere sintering furnace and is calcined, ball mill is sent into and carries out ball mill grinding, obtain grain size in 30 μm of coarse powder below；Coarse powder is subjected to 200 mesh sievings, the powder under sieving is spare powder；Spare powder is carried out according to die size with equal pressing equipment just molded, crude green body thickness is suppressed according to using thickness；Crude green body is fitted into graphite jig, is then packed into vacuum sintering funace and is sintered；After the completion of sintering, cooling pressure release is come out of the stove, and thick target is obtained；Finally finishing obtains molybdenum disulfide target.Manufacturing process of the present invention is simple, easy to operate, safety non-pollution, and the molybdenum disulfide target of preparation is non-conductive, and compactness and stability are good, and surface is smooth, to realize that molybdenum disulfide plated film provides reliable guarantee.
Description
Technical field
The present invention relates to target preparing technical field, especially a kind of preparation method of molybdenum disulfide target.
Background technology
Molybdenum disulfide is important kollag, has excellent greasy property, it is extensive to can be used as kollag
The mechanical lubrication of vacuum lubrication and petrochemical industry applied to aerospace industry.Molybdenum disulfide have good dispersion, not bond,
The advantage that bearing capacity is high, friction factor is low, can add in various greases, inadherent colloidal state absolutely be formed, as solid
Body lubricant can substantially reduce the friction and wear of workpiece surface, improve the service efficiency of workpiece, and extend workpiece uses the longevity
Life, is most wide one of the lubriation material of space precise machine applications, is commonly applied to the fretting wear workpiece and space of vacuum environment
On aircraft, including the vacuum such as satellite movable part and precise rolling bearing lubrication；It also can be applicable to friction material industry simultaneously
In, antifriction when friction material major function is low temperature increases when high temperature and rubs, and loss on ignition is small, volatile in friction material.Certainly,
Molybdenum disulfide also has disadvantage, such as poor thermal conductivity, friction coefficient are not low enough, penetrating power is not strong etc..
With the development of technology, to lubricating and wear-resisting requirement is higher and higher, WeiLai Technology is with greater need for by molybdenum disulfide system
At a kind of heat safe film, to reduce the use of grease, to improve the service life of part of appliance.Coating process compares at present
Advanced and free of contamination technique is magnetron sputtering physical coating technology, and such technique needs the material by plated film with the shape of target
Formula carries out bombardment as carrier, to molybdenum disulfide and completes plated film, therefore to obtain molybdenum disulfide film, then is necessarily required to curing
Molybdenum target material.
Before molybdenum disulfide target is researched and developed successfully, laboratory attempts, using molybdenum target material as base material, to be passed through in coating process
The SO of ratio2Gas carries out reactive sputtering, but this technique requires coating technique high, the uniformity of film not easy to control, at present
It cannot achieve industrialization.Therefore in the actual production process, it is to prepare two as raw material using molybdenum disulfide powder mostly
Vulcanize molybdenum target material, in addition, molybdenum disulfide is a kind of lamella compound with hexagonal system structure, interlayer has weaker model moral
Splitting easily occurs for Hua Li, has good anisotropy and lower friction factor, therefore, how by two loose sulphur
Change molybdenum powder body and carry out compacting sintering molding, becomes insoluble technological difficulties during being prepared for molybdenum disulfide target.
Invention content
The technical problem to be solved in the invention is to provide a kind of preparation method of molybdenum disulfide target, is overcoming traditional work
Skill can not improve compactness, stability and the surface flatness of molybdenum disulfide target on the basis of sinter molding, for can be real
Existing magnetron sputtering plating provides basis.
In order to solve the above technical problems, the technical solution used in the present invention is as follows.
A kind of preparation method of molybdenum disulfide target, includes the following steps：
A, the pretreatment of molybdenum disulfide powder：Molybdenum disulfide powder is put into ball milling with a certain proportion of through magnetized metal material
Machine progress ball milling mixing is uniform, obtains mixed material；
B, the mixed material for obtaining step A carries out isostatic pressing, and hydrostatic pressure is pressed into blocky thick in 100 ~ 125MPa
Base；
C, blocky crude green body obtained by step B being put into atmosphere sintering furnace and is calcined, calcination temperature is 1350 DEG C, keeps the temperature 2 hours,
Power-off cooling, 100 DEG C or less are come out of the stove；
D, the product for obtaining step C is sent into ball mill and carries out ball mill grinding, and Ball-milling Time is 5 hours, obtains grain size at 30 μm
Coarse powder below；
E, the coarse powder for obtaining step D carries out 200 mesh sievings, and the powder under sieving is spare powder；
F, spare powder that step E is obtained is carried out with equal pressing equipment according to die size it is just molded, crude green body thickness according to
It is suppressed using thickness；
G, the step F crude green bodies waited until are fitted into graphite jig, are separated with 10mm thickness molybdenum sheets between adjacent crude green body；Crude green body will be housed
Mold be packed into vacuum sintering funace in be sintered, control 1000 ~ 1050 DEG C of sintering temperature, sintering rate at 5 DEG C/minute,
25 ~ 38MPa of sintering pressure, and 2 ~ 5h of heat-insulation pressure keeping；
H, after the completion of sintering, 500 DEG C are cooled to, pressure release to normal pressure continues to come out of the stove when cooling to 150 DEG C or less, obtains thick target；
I, it finishes：The thick target that step H is obtained obtains molybdenum disulfide target by cutting, flat stone mill processing.
A kind of preparation method of above-mentioned molybdenum disulfide target, it is Ni through magnetized metal material to be added described in step A
Powder and Co powder；Wherein, it is wt%Co=0.5 ~ 3% that the adding proportion of Ni powder, which is the adding proportion of wt%Ni=2 ~ 5%, Co powder,.
A kind of preparation method of above-mentioned molybdenum disulfide target, purity >=99.95%, Ni powder of molybdenum disulfide powder in step A
Purity >=99.95%, Co powder purity >=99.95%.
A kind of preparation method of above-mentioned molybdenum disulfide target, balls are zirconia ball in ball mill described in step D, and ball is big
It is small to be divided into three kinds：Φ 30mm balls account for the one third of ball sum, and Φ 10mm balls account for the one third of ball sum, and Φ 5mm balls account for ball
The one third of sum.
As a result of above technical scheme, the invention technological progress is as follows.
Molybdenum disulfide target is prepared using the present invention, manufacturing process is simple, easy to operate, safety non-pollution, and two prepared
It is non-conductive to vulcanize molybdenum target material, target density >=4.7g/cm3, for compactness up to 98% or more, stability is good, and surface smoothness is good, adds
Heat is not decomposed to 200 DEG C or more targets, is not had gas release, can be realized magnetron sputtering, and sputter the smooth no knot of runway
Tumor, to realize that molybdenum disulfide plated film provides reliable guarantee.Molybdenum disulfide target prepared by the present invention is used as magnetron sputtering plating
Base material improves high temperature resistant, the antiwear characteristic of sealing element, extends, it can be achieved that plate molybdenum disulfide film on the sealing elements such as bearing
The service life and service life of sealing element, while the use of lubricating oil is reduced, reduce pollution.
The present invention controls MoS by adding magnetic material in molybdenum disulfide fission2With the atom number of magnetic material
Than controlling 93.48：6.52 to 80.87：Between 19.13, i.e., there are one magnetic atom, magnetic for meeting averagely between 4 to 13 atoms
Property material under high temperature, high vacuum condition enter molybdenum disulfide lattice in, substitution part molybdenum disulfide member usually reduce curing
The slickness of molybdenum itself realizes the molding of molybdenum disulfide ceramic target.
Specific implementation mode
A kind of preparation method of molybdenum disulfide target is added by being pre-processed to molybdenum disulfide powder through magnetized
After Ni, Co metal material, carry out ball milling mixing makes Ni, Co enter molybdenum disulfide lattice then under high temperature, high vacuum condition
In, replace part molybdenum disulfide element, to reduce the slickness of molybdenum disulfide itself, realize molybdenum disulfide ceramic target at
Type.The preparation method specifically includes following steps.
A, the pretreatment of molybdenum disulfide powder：Molybdenum disulfide powder is put into a certain proportion of through magnetized metal material
Ball mill progress ball milling mixing is uniform, obtains mixed material.It is Ni powder and Co powder through magnetized metal material in the present invention；Wherein,
The adding proportion of Ni powder is that the adding proportion of wt%Ni=2 ~ 5%, Co powder is wt%Co=0.5 ~ 3%.In the raw material of addition, molybdenum disulfide
Purity >=99.95% of purity >=99.95%, Co powder of purity >=99.95%, Ni powder of powder.
Certainly, Ni and Co is all the material magnetized, molecular weight substantially close to（Ni=58.69；Co=58.93）, so adding
Add any one or both of which can be with as long as total amount of adding between 2.5 ~ 8%, i.e., does not influence the performance of molybdenum disulfide target.
The present invention is added to magnetic material in molybdenum disulfide powder, and controls the adding proportion of magnetic material, MoS2
For ratio with magnetic material only within the scope of this, molybdenum disulfide powder can be only achieved balance, if magnetic material added
More, target will have magnetic and metallicity, and the ceramic performance of itself substantially reduces；If addition is very few, moieties
One is not formed, being sintered out target material surface will cracked trace.
B, the mixed material for obtaining step A carries out isostatic pressing, and hydrostatic pressure is in 100 ~ 125MPa, briquet
Shape crude green body.
C, blocky crude green body obtained by step B is put into atmosphere sintering furnace and is calcined, calcination temperature is 1350 DEG C, heat preservation 2
Hour, power-off cooling, 100 DEG C or less are come out of the stove.
D, the product for obtaining step C is sent into ball mill and carries out ball mill grinding, and Ball-milling Time is 5 hours, obtains grain size and exists
30 μm of coarse powder below.The present invention is to ensure that the grain size of coarse powder is met the requirements, and balls are zirconia ball in the ball mill, and ball is big
It is small to be divided into three kinds：Φ 30mm balls account for the one third of ball sum, and Φ 10mm balls account for the one third of ball sum, and Φ 5mm balls account for ball
The one third of sum.
E, the coarse powder for obtaining step D carries out 200 mesh sievings, and the powder under sieving is spare powder.
F, the spare powder that step E is obtained is subjected to just molded, crude green body thickness with equal pressing equipment according to die size
It is suppressed according to thickness is used.
G, the step F crude green bodies waited until are fitted into graphite jig, are separated with 10mm thickness molybdenum sheets between adjacent crude green body；It will be equipped with
The mold of crude green body is packed into vacuum sintering funace and is sintered, and controls 1000 ~ 1050 DEG C of sintering temperature, sintering rate 5 DEG C/
Point, 25 ~ 38MPa of sintering pressure, and 2 ~ 5h of heat-insulation pressure keeping.
In the present invention, vacuum hot-pressed sintered technology is that pressure sintering is carried out under high vacuum, high temperature, due to molybdenum disulfide
Fusing point is at 1180 DEG C, after adding some materials, the principle according to the fusing point of mixture less than the fusing point of any one material, and mixing
Object can reduce the fusing point of material, and again under high vacuum condition, and fusing point is lower than normal pressure-sintered fusing point, so passing through many experiments
It is 1000-1050 DEG C to eventually find suitable sintering temperature point.The setting of pressure is the moulding process according to molybdenum disulfide target
The suitable pressure range that condition is found by many experiments.
H, after the completion of sintering, 500 DEG C are cooled to, pressure release to normal pressure continues to come out of the stove when cooling to 150 DEG C or less, obtains thick
Target.
After target is sintered, temperature needs slowly to reduce, this stage is target sizing formative stage, if being higher than 500
DEG C pressure release, target are easily bent, carry out pressure release again so should be cooled to after 500 DEG C, after the completion of pressure release, continuing to cool to 150
It DEG C comes out of the stove, the setting of this temperature is because burner hearth material is graphite product, and mold is graphite jig, if tapping temperature is excessively high,
Burner hearth and mold will appear oxidative phenomena, reduce the service life of burner hearth and mold.
I, it finishes：The thick target that step H is obtained obtains molybdenum disulfide target by cutting, flat stone mill processing.
Below in conjunction with specific embodiment, the present invention will be described in further detail.
Embodiment 1
A kind of preparation method of molybdenum disulfide target, specifically includes following steps.
A, the pretreatment of molybdenum disulfide powder：Molybdenum disulfide powder is put into a certain proportion of through magnetized metal material
Ball mill progress ball milling mixing is uniform, obtains mixed material.It is Ni powder and Co powder through magnetized metal material in the present embodiment；Its
In, the adding proportion of Ni powder is wt%Ni=3%, and the adding proportion of Co powder is wt%Co=2%.In the raw material of addition, molybdenum disulphide powder
Purity >=99.95% of purity >=99.95%, Co powder of purity >=99.95%, Ni powder of body.
B, the mixed material for obtaining step A carries out isostatic pressing, and hydrostatic pressure is pressed into blocky thick in 125MPa
Base.
C, blocky crude green body obtained by step B is put into atmosphere sintering furnace and is calcined, calcination temperature is 1350 DEG C, heat preservation 2
Hour, power-off cooling, 100 DEG C or less are come out of the stove.
D, the product for obtaining step C is sent into ball mill and carries out ball mill grinding, and Ball-milling Time is 5 hours, obtains grain size and exists
30 μm of coarse powder below.
E, the coarse powder for obtaining step D carries out 200 mesh sievings, and the powder under sieving is spare powder.
F, the spare powder that step E is obtained is subjected to just molded, crude green body thickness with equal pressing equipment according to die size
It is suppressed according to thickness is used.
G, the step F crude green bodies waited until are fitted into graphite jig, are separated with 10mm thickness molybdenum sheets between adjacent crude green body；It will be equipped with
The mold of crude green body is packed into vacuum sintering funace and is sintered, and controls 1000 DEG C of sintering temperature, and sintering rate is burnt at 5 DEG C/minute
Knot pressure power 30MPa, and heat-insulation pressure keeping 4h.
H, after the completion of sintering, 500 DEG C are cooled to, pressure release to normal pressure continues to come out of the stove when cooling to 150 DEG C or less, obtains thick
Target.
I, it finishes：The thick target that step H is obtained obtains molybdenum disulfide target by cutting, flat stone mill processing.
After testing, molybdenum disulfide target density manufactured in the present embodiment is 4.78g/cm3, relative density 98.5%, target
Purity is 99.98%.Target crystalline grains degree is uniform, is 40 ± 2 μm.
Embodiment 2
A kind of preparation method of molybdenum disulfide target, specifically includes following steps.
A, the pretreatment of molybdenum disulfide powder：Molybdenum disulfide powder is put into a certain proportion of through magnetized metal material
Ball mill progress ball milling mixing is uniform, obtains mixed material.It is Ni powder through magnetized metal material in the present embodiment；Wherein, Ni powder
Adding proportion be wt%Ni=5.6%, in the raw material of addition, the purity of purity >=99.95%, Ni powder of molybdenum disulfide powder >=
99.95%。
B, the mixed material for obtaining step A carries out isostatic pressing, and hydrostatic pressure is pressed into blocky thick in 100MPa
Base.
C, blocky crude green body obtained by step B is put into atmosphere sintering furnace and is calcined, calcination temperature is 1350 DEG C, heat preservation 2
Hour, power-off cooling, 100 DEG C or less are come out of the stove.
D, the product for obtaining step C is sent into ball mill and carries out ball mill grinding, and Ball-milling Time is 5 hours, obtains grain size and exists
30 μm of coarse powder below.
E, the coarse powder for obtaining step D carries out 200 mesh sievings, and the powder under sieving is spare powder.
F, the spare powder that step E is obtained is subjected to just molded, crude green body thickness with equal pressing equipment according to die size
It is suppressed according to thickness is used.
G, the step F crude green bodies waited until are fitted into graphite jig, are separated with 10mm thickness molybdenum sheets between adjacent crude green body；It will be equipped with
The mold of crude green body is packed into vacuum sintering funace and is sintered, and controls 1050 DEG C of sintering temperature, and sintering rate is burnt at 5 DEG C/minute
Knot pressure power 38MPa, and heat-insulation pressure keeping 5h.
H, after the completion of sintering, 500 DEG C are cooled to, pressure release to normal pressure continues to come out of the stove when cooling to 150 DEG C or less, obtains thick
Target.
I, it finishes：The thick target that step H is obtained obtains molybdenum disulfide target by cutting, flat stone mill processing.
After testing, molybdenum disulfide target density manufactured in the present embodiment is 4.82g/cm3, relative density 99.1%, target
Purity is 99.96%.Target crystalline grains degree is uniform, is 43 ± 2 μm.
Embodiment 3
A kind of preparation method of molybdenum disulfide target, specifically includes following steps.
A, the pretreatment of molybdenum disulfide powder：Molybdenum disulfide powder is put into a certain proportion of through magnetized metal material
Ball mill progress ball milling mixing is uniform, obtains mixed material.It is Co powder through magnetized metal material in the present embodiment；Co powder adds
It is wt%Co=7% to add ratio.In the raw material of addition, purity >=99.95% of purity >=99.95%, Co powder of molybdenum disulfide powder.
B, the mixed material for obtaining step A carries out isostatic pressing, and hydrostatic pressure is pressed into blocky thick in 110MPa
Base.
C, blocky crude green body obtained by step B is put into atmosphere sintering furnace and is calcined, calcination temperature is 1350 DEG C, heat preservation 2
Hour, power-off cooling, 100 DEG C or less are come out of the stove.
D, the product for obtaining step C is sent into ball mill and carries out ball mill grinding, and Ball-milling Time is 5 hours, obtains grain size and exists
30 μm of coarse powder below.
E, the coarse powder for obtaining step D carries out 200 mesh sievings, and the powder under sieving is spare powder.
F, the spare powder that step E is obtained is subjected to just molded, crude green body thickness with equal pressing equipment according to die size
It is suppressed according to thickness is used.
G, the step F crude green bodies waited until are fitted into graphite jig, are separated with 10mm thickness molybdenum sheets between adjacent crude green body；It will be equipped with
The mold of crude green body is packed into vacuum sintering funace and is sintered, and controls 1020 DEG C of sintering temperature, and sintering rate is burnt at 5 DEG C/minute
Knot pressure power 25MPa, and heat-insulation pressure keeping 3h.
H, after the completion of sintering, 500 DEG C are cooled to, pressure release to normal pressure continues to come out of the stove when cooling to 150 DEG C or less, obtains thick
Target.
I, it finishes：The thick target that step H is obtained obtains molybdenum disulfide target by cutting, flat stone mill processing.
After testing, molybdenum disulfide target density manufactured in the present embodiment is 4.75g/cm3, relative density 98.3%, target
Purity is 99.97%.Target crystalline grains degree is uniform, is 45 ± 2 μm.
Embodiment described above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention.Every basis
Inventive technique essence still falls within skill of the present invention to any simple modification, change and equivalence change made by above example
In the protection domain of art scheme.
Claims (4)
1. a kind of preparation method of molybdenum disulfide target, which is characterized in that include the following steps：
A, the pretreatment of molybdenum disulfide powder：Molybdenum disulfide powder is put into ball milling with a certain proportion of through magnetized metal material
Machine progress ball milling mixing is uniform, obtains mixed material；
B, the mixed material for obtaining step A carries out isostatic pressing, and hydrostatic pressure is pressed into blocky thick in 100 ~ 125MPa
Base；
C, blocky crude green body obtained by step B being put into atmosphere sintering furnace and is calcined, calcination temperature is 1350 DEG C, keeps the temperature 2 hours,
Power-off cooling, 100 DEG C or less are come out of the stove；
D, the product for obtaining step C is sent into ball mill and carries out ball mill grinding, and Ball-milling Time is 5 hours, obtains grain size at 30 μm
Coarse powder below；
E, the coarse powder for obtaining step D carries out 200 mesh sievings, and the powder under sieving is spare powder；
F, spare powder that step E is obtained is carried out with equal pressing equipment according to die size it is just molded, crude green body thickness according to
It is suppressed using thickness；
G, the step F crude green bodies waited until are fitted into graphite jig, are separated with 10mm thickness molybdenum sheets between adjacent crude green body；Crude green body will be housed
Mold be packed into vacuum sintering funace in be sintered, control 1000 ~ 1050 DEG C of sintering temperature, sintering rate at 5 DEG C/minute,
25 ~ 38MPa of sintering pressure, and 2 ~ 5h of heat-insulation pressure keeping；
H, after the completion of sintering, 500 DEG C are cooled to, pressure release to normal pressure continues to come out of the stove when cooling to 150 DEG C or less, obtains thick target；
I, it finishes：The thick target that step H is obtained obtains molybdenum disulfide target by cutting, flat stone mill processing.
2. a kind of preparation method of molybdenum disulfide target according to claim 1, which is characterized in that add described in step A
It is Ni powder and Co powder through magnetized metal material to add；Wherein, the adding proportion of Ni powder is the addition ratio of wt%Ni=2 ~ 5%, Co powder
Example is wt%Co=0.5 ~ 3%.
3. a kind of preparation method of molybdenum disulfide target according to claim 1, which is characterized in that curing in step A
Purity >=99.95% of purity >=99.95%, Co powder of purity >=99.95%, Ni powder of molybdenum powder body.
4. a kind of preparation method of molybdenum disulfide target according to claim 1, which is characterized in that ball milling described in step D
Balls are zirconia ball in machine, and ball size is divided into three kinds：Φ 30mm balls account for the one third of ball sum, and it is total that Φ 10mm balls account for ball
Several one thirds, Φ 5mm balls account for the one third of ball sum.
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| CN115745603A (en) * | 2022-10-17 | 2023-03-07 | 河北东同光电科技有限公司 | Preparation method of large-size high-performance niobium oxide target |
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