CN108103460A - A kind of titanium carbide target and preparation method thereof - Google Patents
A kind of titanium carbide target and preparation method thereof Download PDFInfo
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- CN108103460A CN108103460A CN201711188416.0A CN201711188416A CN108103460A CN 108103460 A CN108103460 A CN 108103460A CN 201711188416 A CN201711188416 A CN 201711188416A CN 108103460 A CN108103460 A CN 108103460A
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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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- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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Abstract
The present invention provides a kind of titanium carbide target and preparation method thereof, and this method is：Pure carbonization titanium material powder is subjected to screening process first, obtains even-grained powder, carries out handling with carbon afterwards, obtains the suitable mixed raw material of ingredient；Then uniformly it is filled into mold, carries out hot pressed sintering processing under vacuum, after cooling, the demoulding obtains sintered blank；Finally sintered blank is machined out to obtain the titanium carbide target for meeting size and surface quality requirements.This method is simple for process, forming effect is preferable, is mass produced beneficial to industrialization；Target is without any cohesive phase constituent, and crystal grain is uniformly tiny, and consistency can reach more than 99%, and purity is more than 99.9%；The target improves in sputtering process and beats arc discharge phenomenon, the film surface defect of preparation is less, and coating is more fine and close, can be used as and prepare titanium carbide coating, coating mechanical property and tribological property are improved, especially suitable for processing the flexible metal materials such as aluminium and aluminium alloy.
Description
Technical field
The invention belongs to target material preparing technical fields, are related to a kind of titanium carbide target and preparation method thereof, party's legal system
Standby target is especially suitable for processing aluminium and aluminium alloy cutter coat.
Background technology
Titanium carbide material is due to its higher hardness, good corrosion resistance, excellent high-temperature oxidation resistance, application
In surface hard coatings art, especially as metals and its alloy material such as titanium carbide coating, processing aluminum bronze is prepared, add
The bond strength of coating improves the mechanical property and tribological property of coating, improves " viscous knife " phenomenon in process.
Titanium carbide material belongs to high hardness material, and the deformability of material is poor, therefore, the solid phase between titanium carbide powder
It is very big to be sintered resistance, in the case where no binding agent adds, it is difficult to obtain high compactedness material of the consistency more than 99%.
In recent years, what research both at home and abroad was most hot is discharge plasma sintering (SPS) technique, is pressed using 1800 DEG C, 35MPa
Power, heat preservation 5min, can obtain the dense sintering body of relative density about 98%, but cannot obtain relative density substantially more than 98%
Sintered body, and SPS sintering test sample size limitations, stability are poor, it is impossible to meet large scale, the industrialized production of mass
It is required that.
SPS techniques are when preparing large scale sample, since the uniformity of temperature is poor, cause the tissue of blank and density equal
Even property is poor.Therefore, be badly in need of it is a kind of prepare large scale, can mass production, consistency be high, tissue and density uniformity are good
The method of titanium carbide target.
The content of the invention
Present invention aims at a kind of titanium carbide target of offer and preparation method thereof, titanium carbide target prepared by this method,
Uniform small grains, sputtering performance are stablized, and satisfaction prepares the requirement of titanium carbide coating, improves the mechanical property of coating and rub
It wipes and learns performance, improve coating " viscous knife " phenomenon.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of titanium carbide target, comprises the following steps successively：
Step 1：Carbonization titanium material powder is subjected to screening process, obtains even-grained titanium carbide powder；
Step 2：The even-grained titanium carbide powder handled with carbon, obtains mixed raw material powder；
The mixed raw material powder is filled uniformly in mold, then carries out hot pressing under vacuum by step 3
Sintering processes obtain sintered blank through cooling down, demoulding；
Step 4: the sintered blank is machined out to obtain the carbonization titanium target for meeting size and surface quality requirements
Material.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 1, the screening process was 80-200 mesh
Sieve, extracting screen underflow, screening process are used for controlling the dispersiveness and break up agglomerates of powder.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 1, the powder of the carbonization titanium material powder takes
Family name's granularity is 1-15 μm, it is highly preferred that purity >=99.9% of the carbonization titanium material powder.Powder size can influence sintered body
Performance, powder size of the invention is easier to obtain dense sintering body.
In above-mentioned preparation method, as a kind of preferred embodiment, any bonding is not contained in the mixed raw material powder
Agent.In the case that one of features of the present invention is during guarantee prepares titanium carbide target without using any binding agent, system
For the target for going out high-compactness, so as to which harmful effect will not be caused to the use of application end.
In above-mentioned preparation method, as a kind of preferred embodiment, it is described with carbon processing be directed to it is described even-grained
Carbon source is added in titanium carbide powder and is uniformly mixed；It is highly preferred that the addition of the carbon source is the even-grained carbonization
The 0.1-3% of titanium powder quality, such as 0.2%, 0.5%, 1%, 2%, 2.5%；It is further preferred that the carbon source is graphite
Powder.In order to reduce the carbon loss in sintering process, while the defects of reduce sintered article, the titanium carbide powder after screening is matched somebody with somebody
Carbon processing, in the mixture of 0.5wt%, (addition of i.e. described carbon source is the even-grained titanium carbide powder matter to mixed carbon comtent
The 0.5% of amount), sintering character is optimal.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 3, the mold is isostatic pressing formed graphite mold
Or charcoal charcoal mold, both molds have better strength character, are less likely to occur to crack in pressing process.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 3, the sintering temperature of the hot pressed sintering processing
It spends for 1800-2100 DEG C (such as 1820 DEG C, 1850 DEG C, 1880 DEG C, 1920 DEG C, 1950 DEG C, 1980 DEG C, 2000 DEG C), compacting pressure
Power be 28-40MPa (such as 28MPa, 30MPa, 32MPa, 34MPa, 38MPa), the heat-insulation pressure keeping time for 60-90min (such as
62min、65min、68min、72min、75min、80min、82min、85min、88min)；It is highly preferred that the hot pressed sintering
The sintering temperature of processing for 1850-1950 DEG C (such as 1855 DEG C, 1860 DEG C, 1880 DEG C, 1900 DEG C, 1920 DEG C, 1940 DEG C,
1945 DEG C), pressing pressure is 30-38MPa (such as 31MPa, 32MPa, 33MPa, 34MPa, 35MPa, 36MPa, 38MPa), is protected
The warm dwell time for 60-80min (such as 62min, 64min, 66min, 68min, 70min, 72min, 74min, 76min,
78min).It is further preferred that the vacuum condition refers to that the vacuum degree for completing the sintering furnace of the hot pressed sintering processing is not low
In 10Pa (such as 0.001Pa, 0.01Pa, 0.1Pa, 2Pa, 5Pa, 6Pa, 7Pa, 8Pa, 9Pa), more preferably not less than 5Pa.
In above-mentioned preparation method, as a kind of preferred embodiment, in the sintering furnace handled for the hot pressed sintering
During furnace temperature is gradually increased to the sintering temperature, when furnace temperature is less than 1500 DEG C, heating rate is 6-10 DEG C/min, in stove
When temperature rises to the sintering temperature by 1500 DEG C, heating rate is 2-5 DEG C/min.The heating rate of different phase is controlled, favorably
In the consistency for increasing sintered body and ensure the uniformity of tissue.It is highly preferred that in the step 3, the sintering is being heated
Before stove, first by vacuum degree control in the stove of the sintering furnace 6.6 × 10-2More than Pa.Condition of high vacuum degree in holding furnace before heating,
Two aspects of reason, first, being beneficial to the use of hot pressing furnace, base vacuum is higher to prevent that carbon felt is protected in graphite heating body and stove
The oxidation loss of sheath；Second is that reducing oxygen content in stove, the oxidation of titanium carbide material is prevented.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 3, the cooling refer to stove it is air-cooled or
It is cooled fast to less than 200 DEG C (such as 200 DEG C, 190 DEG C, 180 DEG C, 160 DEG C, 140 DEG C).
A kind of titanium carbide target, is prepared using the above method, and the crystal grain of the target is uniform, average grain size 1
~15 μm, relative density can reach more than 98%, and purity is more than 99.9%.
Compared with prior art, the beneficial effects of the invention are as follows：
1) preparation method of titanium carbide target provided by the invention, preparation process is simple for process, forming effect is preferable, is beneficial to
Industrialization large-scale production.By the experiment that controls of different temperatures section heating rate, obtained phase structure to be single pure
TiC targets improve in sputtering process and beat arc discharge phenomenon, and the film surface defect of preparation is less, and coating is more fine and close.
2) the titanium carbide target soap-free emulsion polymeization phase that the method for the present invention is prepared.
3) the pure titanium carbide target prepared by the present invention, crystal grain is uniform, and 1~15 μm of average grain size, consistency is reachable
To more than 98%, for purity more than 99.9%, tissue and density uniformity are good.Pure titanium carbide target performance produced by the present invention is steady
It is fixed, as the cutter coat target source material for preparing processing aluminium and aluminium alloy, improve mechanical property and the friction of coating
Performance is learned, improves " viscous knife " phenomenon in coating processes.
4) since the present invention uses hot-pressed sintering furnace to carry out hot pressed sintering, large-size target can be prepared, while can be real
Existing mass production.
Description of the drawings
Fig. 1 is the microstructure photograph of pure TiC targets prepared by embodiment 3.
Specific embodiment
A kind of specific embodiment that the present invention provides the preparation method of titanium carbide target includes the following steps：
Step A：Stock, it is 1-15 μm to select Fisher particle size, and pure titanium carbide powder of the purity more than 99.9% is as former
Feed powder crosses 100 mesh screens, break up agglomerates, raw material dispersion powder, to control the uniformity of powder size, extracting screen underflow after sieving.
Step B：Screenings in step A handled with carbon, mixed carbon comtent for 0.1-3wt% (such as 0.2%,
0.5%, 1%, 2%, 2.5%, 2.9%), high purity graphite powder is selected to be uniformly mixed as carbon source.Mixed carbon comtent refers to graphite
The addition of powder is the percentage of the quality of the titanium carbide powder after the screening used in the step.Preferably, mixed carbon comtent is
0.5-2wt%.
Step C：It is die-filling, by the mixed-powder that step B is obtained according to certain type of feed (such as first by graphite jig with
The region of powder contact position loads powder, and carries out compacting operation, refills centre position region powder, carries out compacting behaviour
Make, be so conducive to the uniformity loaded) uniformly it is filled into graphite jig.It needs to control the uniform of filling powder during filling
Property, if the uniformity of dress powder is poor, it is easy to cause the Density inhomogeneity of compacting blank；Above-mentioned graphite jig be preferably etc. it is quiet
Graphite jig is pressed, strength character is more preferable, is less likely to occur to crack in pressing process, can be with except isostatic pressing formed graphite mold
Select charcoal charcoal mold.
Step D：Hot pressed sintering, the graphite jig for having been charged into mixed-powder that step C is obtained are positioned over hot-pressed sintering furnace
It is interior, carry out hot pressed sintering；Hot pressed sintering temperature between 1800-2100 DEG C (such as 1820 DEG C, 1850 DEG C, 1880 DEG C, 1920 DEG C,
1950 DEG C, 1980 DEG C, 2000 DEG C), pressing pressure between 28-40MPa (such as 26MPa, 28MPa, 30MPa, 32MPa,
34MPa), sintering temperature and pressing pressure keep 60-90min (such as 62min, 65min, 68min, 72min, 75min,
80min、82min、85min、88min)。
Step E：The demoulding, sintering finish rear mold with stove it is air-cooled or add in fast cooling device, be cooled to less than 200 DEG C (compare
Such as 200 DEG C, 190 DEG C, 180 DEG C, 160 DEG C, 140 DEG C), it is then demoulded, obtains blank；
Step F：Blank using processing methods such as wire cutting, scroll saw, grinding machines is processed and meets client's ruler by following process
Very little and surface quality requirements finished products.
Present disclosure will be described in further detail by embodiment combination attached drawing below, protection of the invention
Scope is including but not limited to following each embodiments.
Specific experiment step or condition are not specified in embodiment, according to the described routine experiment step of document in the art
Operation or condition can carry out.The carbonization titanium material powder used in embodiment be using this field customary preparation methods prepare or
Person uses commercial product, the purity more than 99.9% for the titanium material powder that is carbonized, wherein, total carbon content 6.12wt%, free carbon
Content 0.04wt%.
Embodiment 1-14
Table 1 lists raw material composition, the preparation technology parameter of embodiment 1-14, and specific preparation process is as follows：
(1) stock up, by it is above-mentioned it is pure carbonization titanium material powder cross 100 mesh sieves, take minus sieve powder in next step, minus sieve powder
Fisher particle size can control the uniformity of powder size referring to table 1, screening；
(2) with carbon, above-mentioned steps (1) powder handle with carbon, and be uniformly mixed, wherein, the graphite powder of addition is
The percentage of the titanium carbide powder quality used referring to table 1 mixed carbon comtent；
(3) die-filling, the mixed-powder filling even obtained to step (2) enters in isostatic pressing formed graphite mold；
(4) the isostatic pressing formed graphite mold for having been charged into mixed-powder in step (3) is positioned over hot pressing furnace by hot pressed sintering
It is interior, below 5Pa is evacuated to, then heats to sintering temperature (heating rate is referring to the following table 1), carries out hot pressed sintering, it is specific to burn
Junction parameter is shown in Table 1；
(5) demoulding, it is air-cooled with stove that sintering finishes rear mold, after waiting in-furnace temperatures less than 200 DEG C, the demoulding of coming out of the stove；
(6) machine, blank is processed using processing methods such as wire cutting, scroll saw, grinding machines, reaches surface smoothness
Ra 1.6。
Raw material composition, the preparation technology parameter of 1 embodiment 1-14 of table
The consistency of target is tested by Archimedes's drainage mensuration；The purity of target is tested by GDMS methods；It is logical
The crystallite dimension of nodal method test target is crossed, Fig. 1 is that the scanning electron microscope (SEM) of pure TiC targets prepared by embodiment 3 is shone
Piece, material structure is uniform as can be seen from this figure, for single TiC phases, 15.4 μm of average grain size.
In addition, by sputtering experiment test target as sputter performance：Using magnetron sputtering apparatus, the plated film for carrying out target is real
It tests, selects same plated film laboratory parameters, vacuum degree 5.0 × 10-1, power density 12W/cm2.Target prepared by embodiment 1-14
Performance be shown in Table 2, the stable discharge time is needing the empty time burnt into before stablizing plated film for target；
The stable discharge time refers to that sky burns the time, and " burn in time ", target is before the requirement of deposition film is reached
The time of (electric discharge (arc) frequency reaches certain value) empty sputtering.The stable discharge time is smaller, illustrates target consistency higher, group
It is more excellent to knit uniformity, phase structure is consistent.Discharge time longer explanation, hole, field trash inside target, nonconducting oxidation
The defects of object, is more, and object phase and structural homogenity are poor.
The measure of Coating Surface Roughness is carried out using surface profiler or atomic force microscope.
The target performance parameter of 2 embodiment 1-14 of table
Data can be seen that from the table：1) since above-described embodiment is by raw material control and vacuum hot-pressed sintered technology
The potential risk for increasing impurity element is not present in the TiC targets of preparation, centre, and target purity can be maintained at more than 99.9%；
2) decarburization be easy to cause local grain abnormal growth, in application sputtering process, easily forms electric discharge phenomena, the painting to preparation
Layer surface roughness will also result in large effect；3) preparation parameter with sintering temperature in 1800-1850 DEG C, heat-insulation pressure keeping time
In 75min, pressure is preferred in 38MPa.
Embodiment 15-18
Embodiment 15-18 is in addition to the technological parameter in table 3 is different from embodiment 1, other are same as Example 1, four
The target performance test methods that embodiment obtains are with embodiment 1, as a result referring to table 4.
The technological parameter of 3 embodiment 15-18 of table
The performance for the target that 4 embodiment 15-18 of table is obtained
Claims (10)
1. a kind of preparation method of titanium carbide target, which is characterized in that comprise the following steps successively：
Step 1：Carbonization titanium material powder is subjected to screening process, obtains even-grained titanium carbide powder；
Step 2：The even-grained titanium carbide powder handled with carbon, obtains mixed raw material powder；
The mixed raw material powder is filled uniformly in mold, then carries out hot pressed sintering under vacuum by step 3
Processing, sintered blank is obtained through cooling down, demoulding；
Step 4: the sintered blank is machined out to obtain the titanium carbide target for meeting size and surface quality requirements.
2. preparation method according to claim 1, which is characterized in that in step 1, the screening process was 80-200
Mesh screen, extracting screen underflow.
3. preparation method according to claim 1, which is characterized in that in step 1, the powder of the carbonization titanium material powder
Fisher particle size is 1-15 μm, it is highly preferred that purity >=99.9% of the carbonization titanium material powder.
4. preparation method according to claim 1, which is characterized in that do not contain any bonding in the mixed raw material powder
Agent.
5. according to claim 1-4 any one of them preparation methods, which is characterized in that described to be directed to the grain with carbon processing
It spends in uniform titanium carbide powder and adds in carbon source and be uniformly mixed；Preferably, the addition of the carbon source is the epigranular
Titanium carbide powder quality 0.1-3%；It is further preferred that the carbon source is graphite powder.
6. preparation method according to claim 1, which is characterized in that in step 3, the mold is isostatic pressing formed graphite mould
Tool or charcoal charcoal mold.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that in step 3, at the hot pressed sintering
The sintering temperature of reason is 1800-2100 DEG C, pressing pressure 28-40MPa, and the heat-insulation pressure keeping time is 60-90min；It is highly preferred that
The sintering temperature of the hot pressed sintering processing is 1850-1950 DEG C, pressing pressure 30-38MPa, and the heat-insulation pressure keeping time is 60-
80min.It is further preferred that the vacuum degree that the vacuum condition refers to complete the sintering furnace of the hot pressed sintering processing is not less than
10Pa。
8. preparation method according to claim 7, which is characterized in that in the sintering furnace handled for the hot pressed sintering
During furnace temperature is gradually increased to the sintering temperature, when furnace temperature is less than 1500 DEG C, heating rate is 6-10 DEG C/min, in stove
When temperature rises to the sintering temperature by 1500 DEG C, heating rate is 2-5 DEG C/min, it is highly preferred that in the step 3, is being added
Before the heat sintering furnace, first by vacuum degree control in the stove of the sintering furnace 6.6 × 10-2More than Pa.
9. preparation method according to claim 1, which is characterized in that in step 3, it is described cooling refer to stove it is air-cooled or
Person is cooled fast to less than 200 DEG C.
10. a kind of titanium carbide target is prepared using any the methods of claim 1-9, the crystal grain of the target is uniform,
1~15 μm of average grain size, relative density more than 98%, purity is more than 99.9%.
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| CN201711188416.0A CN108103460B (en) | 2017-11-24 | 2017-11-24 | A kind of titanium carbide target and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773084A (en) * | 2021-09-08 | 2021-12-10 | 宁波江丰电子材料股份有限公司 | Tungsten carbide target material for decorative coating and preparation method thereof |
| CN113981388A (en) * | 2021-10-25 | 2022-01-28 | 北京安泰六九新材料科技有限公司 | Preparation method of high-density TiAl and TiAlMe target material |
| CN116477626A (en) * | 2023-03-22 | 2023-07-25 | 常熟市电力耐磨合金铸造有限公司 | Superfine TiC powder with low oxygen content and preparation method thereof |
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| CN102699325A (en) * | 2012-06-20 | 2012-10-03 | 江苏美特林科特殊合金有限公司 | Preparing method for Ti-Si alloy target materials |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| TW201602052A (en) * | 2014-03-26 | 2016-01-16 | Jx Nippon Mining & Metals Corp | Sputtering target comprising tungsten carbide or titanium carbide |
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| CN102002605A (en) * | 2010-12-06 | 2011-04-06 | 西安瑞福莱钨钼有限公司 | Preparation method of tungsten titanium alloy plate for sputtering target |
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| CN113773084A (en) * | 2021-09-08 | 2021-12-10 | 宁波江丰电子材料股份有限公司 | Tungsten carbide target material for decorative coating and preparation method thereof |
| CN113981388A (en) * | 2021-10-25 | 2022-01-28 | 北京安泰六九新材料科技有限公司 | Preparation method of high-density TiAl and TiAlMe target material |
| CN116477626A (en) * | 2023-03-22 | 2023-07-25 | 常熟市电力耐磨合金铸造有限公司 | Superfine TiC powder with low oxygen content and preparation method thereof |
| CN116477626B (en) * | 2023-03-22 | 2024-09-24 | 常熟市电力耐磨合金铸造有限公司 | Superfine TiC powder with low oxygen content and preparation method thereof |
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| Publication number | Publication date |
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| CN108103460B (en) | 2019-11-29 |
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