CN100457965C - Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing - Google Patents
Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing Download PDFInfo
- Publication number
- CN100457965C CN100457965C CNB2006101141144A CN200610114114A CN100457965C CN 100457965 C CN100457965 C CN 100457965C CN B2006101141144 A CNB2006101141144 A CN B2006101141144A CN 200610114114 A CN200610114114 A CN 200610114114A CN 100457965 C CN100457965 C CN 100457965C
- Authority
- CN
- China
- Prior art keywords
- thin plate
- silicon
- low
- magnetron sputtering
- silicon steel
- 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.)
- Expired - Fee Related
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The continuous magnetically controlled sputtering and physically vapor depositing process of preparing Fe-6.5 wt%Si sheet includes the first sputtering with monocrystalline or polycrystalline silicon as the cathode target and low silicon steel strap as the anode to deposit silicon substance on single or double sides of the steel strap, and the subsequent high temperature inward diffusing of silicon atoms until reaching the total silicon content of 6.5 wt % and obtaining high silicon steel strap with excellent soft magnetic performance. The present invention has high work efficiency, easy control of the technological parameters and high product quality, and is suitable for industrial application.
Description
Technical field
The present invention relates to a kind of method of the Fe-Si of preparation thin plate, more particularly say, be meant that one adopts the continuous magnetron sputtering physical vaporous deposition to prepare high-quality Fe-5.5~6.7wt%Si thin plate.
Background technology
At present, adopt chemical gaseous phase depositing process and rolling preparation basically about the Fe-6.5wt%Si thin plate in the world.Chemical gaseous phase depositing process is to introduce silane gas in vacuum chamber, by heating silane gas is decomposed after, a certain amount of silicon of deposition on the silicon steel sheet that has carried out suitable pre-treatment; And then, obtain uniform Fe-6.5wt%Si thin plate by thermal treatment.Rolling rule is that direct ingot casting to Fe-6.5wt%Si carries out heat, cold repeatedly rolling, obtains the thin plate of desired thickness.Because the fragility of Fe-6.5wt%Si self and the restriction on the rolling technology, the Fe-6.5wt%Si sheet gauge of rolling preparation generally is difficult to be lower than 0.30mm, and cost is higher.Therefore, present commercial Fe-6.5wt%Si thin plate adopts the chemical gaseous phase depositing process preparation basically, and its thickness is generally 0.10~0.35mm.
The Fe-6.5wt%Si thin plate of chemical gaseous phase depositing process preparation has that cost is low, thickness can reach 0.10mm, be applicable to characteristics such as mass production, but also have surface quality poor, easily introduce impurity and reduce magnetic property, equipment life low, need problem such as environmental protection treatment.
Notification number CN 1200128C discloses a kind of method that adopts discharge plasma sintering to prepare the Fe-6.5wt%Si composite block material with plastic deformation ability.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts the continuous magnetron sputtering physical vapor deposition to prepare Fe-5.5~6.7wt%Si thin plate, this magnetron sputtering physical gas-phase deposite method makes the Ar atomic ionization under vacuum, electric field action, by Ar ion bombardment target Si, with the Si sputtering sedimentation to the low-silicon steel substrate surface, and then pass through High temperature diffusion, realization is handled the siliconising of low-silicon steel band, obtains a kind of preparation method of novel Fe-5.5~6.7wt%Si thin plate.
The present invention is that a kind of employing continuous magnetron sputtering physical vapor deposition prepares Fe-5.5~6.7wt%Si thin plate method, and it has the following step:
Step 1: the low-silicon steel band of choosing thickness and be 0.1~0.35mm is made substrate
Elder generation is dilute hydrochloric acid cleaning 3~10min of 4~10% with concentration;
Be that 75% alcohol cleans 5~10min with concentration again, dry up stand-by;
Step 2: choose silicon Si target
Choose the silicon Si of 200~300mm * 100~150mm * 2~5mm, stand-by;
Step 3: the low-silicon steel band after step 1 is handled is installed on the positive plate of magnetic control sputtering device; Again the silicon Si target after step 2 is handled is put into magnetic control sputtering device, as negative electrode;
Suction to 10
-2~10
-3Behind the Pa, feed argon gas and make pressure-stabilisation in the magnetic control sputtering device in 1~10Pa scope;
Regulate magnetron sputtering codeposition condition:
The preheating low-silicon steel brings to 500 ℃~800 ℃;
Sparking voltage 280V~350V, electric current 0.2A~0.6A, sedimentation rate are 0.5~1.2 μ m/min;
Under this condition, carry out low-silicon steel belt surface silicon deposited film, prepare the plated film steel band;
Step 4: the plated film steel band after step 3 is handled is carried out 1000~1250 ℃ of High temperature diffusion, and diffusion time, 5~60min promptly obtained the uniform Fe-5.5 of section composition~6.7wt%Si thin plate material.
The present invention adopts the continuous magnetron sputtering physical vapor deposition to prepare Fe-5.5~6.7wt%Si thin plate method and chemical Vapor deposition process compares, and magnetron sputtering method has deposition Si purity height, controllable component; Its post-depositional surface quality is good and even; Characteristics such as magnetron sputtering siliconising process controllability is strong, the feature of environmental protection is good.
It is 5.5~6.7% through the Si content that EDS energy spectrometer and electron probe micro-analysis line sweep detect sample that Fe-5.5~6.7wt%Si thin plate that the present invention adopts the continuous magnetron sputtering physical vapor deposition to prepare has (1), and Si content deposition presents uniform distribution; (2) its soft magnetic performance: B after testing
8=1.15T~1.30T, Hc=0.2~0.8Oe, P
10/50=0.50W/kg~0.88W/kg, P
10/400=7.00W/kg~11.35W/kg.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
The step that the present invention adopts the continuous magnetron sputtering physical vapor deposition to prepare Fe-5.5~6.7wt%Si thin plate method has:
Step 1: the low-silicon steel band of choosing thickness and be 0.1~0.35mm is as substrate
Elder generation is dilute hydrochloric acid cleaning 3~10min of 4~10% with concentration;
Be that 75% alcohol cleans 5~10min with concentration again, dry up stand-by;
Step 2: choose silicon Si target
Choose the silicon Si of 200~300mm * 100~150mm * 2~5mm, stand-by;
Step 3: the low-silicon steel band after step 1 is handled is installed on the positive plate of magnetic control sputtering device; Again the silicon Si target after step 2 is handled is put into magnetic control sputtering device, as negative electrode;
Suction to 10
-2~10
-3Behind the Pa, feed argon gas and make pressure-stabilisation in the magnetic control sputtering device in 1~10Pa scope;
Regulate magnetron sputtering codeposition condition:
The preheating low-silicon steel brings to 500 ℃~800 ℃;
Sparking voltage 280V~350V, electric current 0.2A~0.6A, sedimentation rate are 0.5~1.2 μ m/min;
Under this condition, carry out low-silicon steel belt surface silicon deposited film, prepare the plated film steel band;
In this step, low-silicon steel belt surface silicon deposited film thickness can be 5~20 μ m, can obtain the concrete siliconising time by deposition different thickness rete.
In this step, can be placed on respectively by silicon Si target on two target platforms in the magnetic control sputtering device two identical components, be implemented in the substrate above and below and carry out synchronous siliconising processing.Promptly select for use two cathode targets to realize the sputter of synchronous double-side silicon.
Step 4: the plated film steel band after step 3 is handled is carried out 1000~1250 ℃ of High temperature diffusion, and diffusion time, 5~60min promptly obtained the uniform Fe-5.5 of section composition~6.7wt%Si thin plate material.
Fe-5.5~6.7wt%Si thin plate material is detected through EDS energy spectrometer and electron probe micro-analysis line sweep, and its Si content presents uniform distribution.Its soft magnetic performance: B after testing
8=1.15T~1.30T, Hc=0.2~0.8Oe, P
10/50=0.50W/kg~0.88W/kg, P
10/400=7.00W/kg~11.35W/kg.
The present invention adopts the continuous magnetron sputtering physical vapor deposition to prepare Fe-5.5~6.7wt%Si thin plate method, can continuously, controllably carry out siliconising and handle on technology.By to the choosing of a plurality of target platforms in the magnetic control sputtering device, can carry out the deposition of single face and/or two-sided Si arbitrarily, also can regulate simultaneously sedimentation rate, its depositing operation is simple to operate.
In the present invention, selecting the fair low-silicon steel is the siliconising substrate, and its Si content is 2~5wt%.The low-silicon steel of choosing different Si content carries out repeatedly siliconising experiment for the siliconising substrate, and the result shows, after method of the present invention is handled, can obtain Fe-5.5~6.7wt%Si thin plate.
To enumerate three examples below and continuous magnetron sputtering physical vapor deposition of the present invention is prepared Fe-5.5~6.7wt%Si thin plate method carry out detailed specific description, handle the scope that belongs to patent application protection of the present invention for the siliconising that the substrate of choosing different Si content adopts the inventive method to carry out.
Embodiment 1The siliconising of magnetron sputtering vapour deposition single face
Step 1: choose wide 200mm, thick 0.35mm, Si content are that the low-silicon steel band of 3.1wt% is made substrate, are earlier 4% dilute hydrochloric acid cleaning 10min with concentration; Be that 75% alcohol cleans 5min with concentration again, dry up stand-by;
Step 2: choose polysilicon Si target
Choose the polysilicon Si of 200mm * 100mm * 3mm, stand-by;
Step 3: the low-silicon steel band after step 1 is handled is installed on the positive plate of magnetic control sputtering device; Again the polysilicon Si target after step 2 is handled is put into magnetic control sputtering device, as negative electrode;
Suction to 10
-3Behind the Pa, feed argon gas and make pressure-stabilisation in the magnetic control sputtering device at 1Pa;
Regulate magnetron sputtering codeposition condition:
The preheating low-silicon steel brings to 800 ℃;
Sparking voltage 320V, electric current 0.3A, sedimentation rate are 0.5~1.2 μ m/min;
Carry out low-silicon steel belt surface siliceous deposits under this condition, preparing thicknesses of layers is the plated film steel band of 15 μ m;
Step 4: the plated film steel band after step 3 is handled is carried out 1150 ℃ of High temperature diffusion, and be 30min diffusion time, promptly obtains the uniform Fe-5.5 of section composition~6.7wt%Si thin plate material.
Is 6.50wt% with the above-mentioned Fe-5.5 for preparing~6.7wt%Si thin plate through the Si content that EDS energy spectrometer and electron probe micro-analysis line sweep detect sample, presents uniform distribution.Its soft magnetic performance B after testing
8=1.22T, Hc=0.4Oe, P
10/50=0.53W/kg, P
10/400=7.35W/kg.
Embodiment 2The siliconising of magnetron sputtering vapour deposition single face
Step 1: choose wide 200mm, thick 0.35mm, Si content are that the low-silicon steel band of 2.8wt% is made substrate, are earlier 4% dilute hydrochloric acid cleaning 10min with concentration; Be that 75% alcohol cleans 5min with concentration again, dry up stand-by;
Step 2: choose silicon single crystal Si target
Choose the silicon single crystal Si of 200mm * 100mm * 3mm, stand-by;
Step 3: the low-silicon steel band after step 1 is handled is installed on the positive plate of magnetic control sputtering device; Again the silicon single crystal Si target after step 2 is handled is put into magnetic control sputtering device, as negative electrode;
Suction to 10
-2Behind the Pa, feed argon gas and make pressure-stabilisation in the magnetic control sputtering device at 2Pa;
Regulate magnetron sputtering codeposition condition:
The preheating low-silicon steel brings to 650 ℃;
Sparking voltage 350V, electric current 0.25A, sedimentation rate are 0.5~1.2 μ m/min;
Carry out low-silicon steel belt surface siliceous deposits under this condition, preparing thicknesses of layers is the plated film steel band of 20 μ m;
Step 4: the plated film steel band after step 3 is handled is carried out 1200 ℃ of High temperature diffusion, and be 20min diffusion time, promptly obtains the uniform Fe-5.5 of section composition~6.7wt%Si thin plate material.
Is 6.51wt% with the above-mentioned Fe-5.5 for preparing~6.7wt%Si thin plate through the Si content that EDS energy spectrometer and electron probe micro-analysis line sweep detect sample, after testing its soft magnetic performance B
8=1.28T, Hc=0.3mOe, P
10/50=0.51W/kg, P
10/400=7.38W/kg.
Embodiment 3The two-sided siliconising of magnetron sputtering vapour deposition
Step 1: choose wide 200mm, thick 0.35mm, Si content are that the low-silicon steel band of 3.1wt% is made substrate, are earlier 4% dilute hydrochloric acid cleaning 10min with concentration; Be that 75% alcohol cleans 5min with concentration again, dry up stand-by;
Step 2: choose polysilicon Si target
Choose the polysilicon Si of two 200mm * 100mm * 3mm, stand-by;
Step 3: the low-silicon steel band after step 1 is handled is installed on the positive plate of magnetic control sputtering device; Again the polysilicon Si target after step 2 is handled is put into respectively on two target platforms of magnetic control sputtering device, as negative electrode;
Suction to 10
-3Behind the Pa, feed argon gas and make pressure-stabilisation in the magnetic control sputtering device at 1Pa;
Regulate magnetron sputtering codeposition condition:
The preheating low-silicon steel brings to 800 ℃;
Sparking voltage 280V, electric current 0.3A, sedimentation rate are 0.5~1.2 μ m/min;
Under this condition, carry out synchronous siliceous deposits, prepare the plated film steel band that thicknesses of layers up and down is 10 μ m the low-silicon steel band is two-sided;
Step 4: the plated film steel band after step 3 is handled is carried out 1150 ℃ of High temperature diffusion, and diffusion time, 15min promptly obtained the uniform Fe-5.5 of section composition~6.7wt%Si thin plate material.
The above-mentioned Fe-5.5 for preparing~6.7wt%Si thin plate is detected the Si content 6.53% of sample through EDS energy spectrometer and electron probe micro-analysis line sweep, present uniform distribution.Its soft magnetic performance B after testing
8=1.23T, Hc=0.25Oe, P
10/50=0.52W/kg, P
10/400=7.3W/kg.
The present invention adopts carries out two-sided synchronous continuous magnetron sputtering preparation method to the low-silicon steel plate and prepares the thick Fe-5.5 of 0.35mm~6.7wt%Si thin plate, can be controlled at the deposition procedures of finishing siliconising in 8~20min.And its uniform deposition area also can satisfy the industrial continuous preparation requirement of Fe-5.5~6.7wt%Si thin plate fully, for the final magnetron sputtering method of realizing prepares Fe-5.5~6.7wt%Si thin plate in industrialization, tinuous production has been established good basis.
Fe-5.5~6.7wt%Si silicon steel has excellent soft magnetic performance, as: the medium-high frequency iron loss is low, magnetic hysteresis flexiblely is zero, coercive force is little, magnetic permeability and saturation induction density are high, is a kind of very outstanding soft magnetic materials.
Claims (5)
1, a kind of employing continuous magnetron sputtering physical vapor deposition prepares Fe-5.5~6.7wt%Si thin plate method, it is characterized in that the following step is arranged:
Step 1: the low-silicon steel band of choosing thickness and be 0.1~0.35mm is made substrate
Elder generation is dilute hydrochloric acid cleaning 3~10min of 4~10% with concentration;
Be that 75% alcohol cleans 5~10min with concentration again, dry up stand-by;
Step 2: choose the Si target
Choose the Si of 200~300mm * 100~150mm * 2~5mm, stand-by;
Step 3: the low-silicon steel band after step 1 is handled is installed on the positive plate of magnetic control sputtering device; Again the Si target after step 2 is handled is put into magnetic control sputtering device, as negative electrode;
Suction to 10
-2~10
-3Behind the Pa, feed argon gas and make pressure-stabilisation in the magnetic control sputtering device in 1~10Pa scope;
Regulate magnetron sputtering codeposition condition:
The preheating low-silicon steel brings to 500 ℃~800 ℃;
Sparking voltage 280V~350V, electric current 0.2A~0.6A, sedimentation rate are 0.5~1.2 μ m/min;
Under this condition, carry out low-silicon steel belt surface silicon deposited film, prepare the plated film steel band;
Step 4: the plated film steel band after step 3 is handled is carried out 1000~1250 ℃ of High temperature diffusion, and diffusion time, 5~60min promptly obtained the uniform Fe-5.5 of section composition~6.7wt%Si thin plate material.
2, employing continuous magnetron sputtering physical vapor deposition according to claim 1 prepares Fe-5.5~6.7wt%Si thin plate method, it is characterized in that: in step 3, select for use two cathode targets to realize the sputter of synchronous double-side silicon.
3, employing continuous magnetron sputtering physical vapor deposition according to claim 1 prepares Fe-5.5~6.7wt%Si thin plate method, it is characterized in that: in step 3, low-silicon steel belt surface silicon deposited film thickness is 5~20 μ m.
4, employing continuous magnetron sputtering physical vapor deposition according to claim 1 prepares Fe-5.5~6.7wt%Si thin plate method, it is characterized in that: the Si target is silicon single crystal or polysilicon.
5, employing continuous magnetron sputtering physical vapor deposition according to claim 1 prepares Fe-5.5~6.7wt%Si thin plate method, it is characterized in that: the B of the Fe-5.5 for preparing~6.7wt%Si thin plate
8=1.15T~1.30T, Hc=0.2~0.8Oe, P
10/50=0.50W/kg~0.88W/kg, P
10/400=7.00W/kg~11.35W/kg.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2006101141144A CN100457965C (en) | 2006-10-30 | 2006-10-30 | Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2006101141144A CN100457965C (en) | 2006-10-30 | 2006-10-30 | Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1944706A CN1944706A (en) | 2007-04-11 |
CN100457965C true CN100457965C (en) | 2009-02-04 |
Family
ID=38044354
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2006101141144A Expired - Fee Related CN100457965C (en) | 2006-10-30 | 2006-10-30 | Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100457965C (en) |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102208237A (en) * | 2010-03-29 | 2011-10-05 | 深圳市铂科磁材有限公司 | Nano ferrosilicon soft magnetic material |
CN102485955A (en) * | 2010-12-02 | 2012-06-06 | 兰州大成科技股份有限公司 | Method for preparing thin silicon steel strip through vacuum film plating |
CN102260874B (en) * | 2011-07-22 | 2013-03-27 | 北京航空航天大学 | Gradient iron silicon alloy with different silicon content distribution and preparation method of gradient iron silicon alloy |
CN102978569B (en) * | 2012-12-18 | 2014-01-22 | 兰州大成科技股份有限公司 | Method for preparing alloy thin plate with Fe, 5.5-6.5% by weight of Si and 0.3-1.0% by weight of Al by adopting continuous multi-arc ion plating physical vapor deposition |
CN103320737B (en) * | 2013-06-26 | 2016-01-13 | 上海大学 | Hot dip process silicon process prepares method and the silicon strip continuous preparation device of high-silicon steel thin strip |
CN104451372B (en) * | 2014-11-26 | 2017-03-15 | 东北大学 | A kind of preparation method of the high silicon non-oriented silicon steel plate of high magnetic strength |
CN110004419B (en) * | 2019-02-28 | 2020-10-30 | 武汉理工大学 | Method for preparing Fe-Si film by utilizing unbalanced magnetron sputtering technology |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11286775A (en) * | 1998-04-02 | 1999-10-19 | Kawasaki Steel Corp | Production of ultralow core loss grain-oriented silicon steel sheet |
JPH11323511A (en) * | 1998-05-18 | 1999-11-26 | Kawasaki Steel Corp | Silicon steel sheet low in residual magnetic flux density and excellent in high frequency core loss characteristic |
JP2000026968A (en) * | 1998-07-08 | 2000-01-25 | Kawasaki Steel Corp | Formation of high-tensile film on grain oriented silicon steel sheet and forming device |
CN1434144A (en) * | 2003-01-28 | 2003-08-06 | 武汉理工大学 | Method for preparing Fe-6.5 wt%Si compound block material with plasticity deformability |
-
2006
- 2006-10-30 CN CNB2006101141144A patent/CN100457965C/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11286775A (en) * | 1998-04-02 | 1999-10-19 | Kawasaki Steel Corp | Production of ultralow core loss grain-oriented silicon steel sheet |
JPH11323511A (en) * | 1998-05-18 | 1999-11-26 | Kawasaki Steel Corp | Silicon steel sheet low in residual magnetic flux density and excellent in high frequency core loss characteristic |
JP2000026968A (en) * | 1998-07-08 | 2000-01-25 | Kawasaki Steel Corp | Formation of high-tensile film on grain oriented silicon steel sheet and forming device |
CN1434144A (en) * | 2003-01-28 | 2003-08-06 | 武汉理工大学 | Method for preparing Fe-6.5 wt%Si compound block material with plasticity deformability |
Also Published As
Publication number | Publication date |
---|---|
CN1944706A (en) | 2007-04-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100457965C (en) | Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing | |
EP3121823B1 (en) | Method for preparing grain boundary diffused rare earth permanent magnetic material by vapor deposition using composite target | |
Jing et al. | Titanium film deposition by high-power impulse magnetron sputtering: Influence of pulse duration | |
CN103726026B (en) | Oxide ceramics target magnetic control sputtering is adopted to prepare the method for film | |
CN105331942B (en) | Yttrium-iron garnet thin film material and preparation method thereof | |
JPS5934421B2 (en) | Thin film manufacturing method | |
CN101319306B (en) | Industrial production system for producing high-silicon strip with magnetron sputtering continuous two-sided codeposition process | |
CN105441877B (en) | The technique that resistance-type thermal evaporation prepares ferrimagnet Fe3Si films | |
CN116288201A (en) | Iron-carbon alloy target and film preparation method thereof | |
CN108085650A (en) | A kind of method that magnetron sputtering prepares high quality bismuth ferrite ferroelectricity photovoltaic film | |
CN103215556A (en) | Rapid deposition process for combined-type spectrally selective absorption film layer | |
CN102817004A (en) | Method for preparing nanometer silicon film through intermediate-frequency magnetron sputtering process, and its special device | |
CN102154621A (en) | Method for preparing Ni-doped AlN-based diluted magnetic semiconductor thin-film material | |
Xia et al. | On the influence of local oxygen addition on the growth of sputter deposited yttrium oxide thin films | |
CN115652267A (en) | Preparation method of TiCrAlNbSi alloy high-temperature oxidation resistant coating | |
CN101736324A (en) | Microwave plasma preparation method of superhard titanium nitride thin film | |
CN102485955A (en) | Method for preparing thin silicon steel strip through vacuum film plating | |
TWI719346B (en) | Apparatus of reactive cathodic arc evaporator for plating lithium-compound thin film and method thereof | |
CN1124364C (en) | Process for preparing ultra-thin silicon nitride film by electron cyclone, resonance, microwave and plasma | |
CN114672778A (en) | Nanocrystalline NbMoTaWTi refractory high-entropy alloy coating and preparation method thereof | |
CN102140621A (en) | Preparation method of dense composite titanium dioxide film | |
Yin et al. | Middle-frequency magnetron sputtering for GaN growth | |
CN110965023A (en) | Titanium nitride film deposition method | |
WO2013087561A2 (en) | ELECTRICALLY CONDUCTIVE SINx CERAMIC METAL COMPOSITE; ITS SPUTTERING TARGETS AND METHODS THEREOF | |
CN101775579B (en) | Preparation method of microwave plasma of titanium dioxide film |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090204 Termination date: 20131030 |