CN107604325A - A kind of preparation method for the DLC film material that radiates - Google Patents
A kind of preparation method for the DLC film material that radiates Download PDFInfo
- Publication number
- CN107604325A CN107604325A CN201710784628.9A CN201710784628A CN107604325A CN 107604325 A CN107604325 A CN 107604325A CN 201710784628 A CN201710784628 A CN 201710784628A CN 107604325 A CN107604325 A CN 107604325A
- Authority
- CN
- China
- Prior art keywords
- film material
- dlc film
- preparation
- radiates
- parts
- 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.)
- Pending
Links
Abstract
The invention discloses a kind of preparation method for the DLC film material that radiates, technology utilization 25%H2O2Handle film-substrate, nickel powder, ethyl acetate, tetrahydrofuran, pentyl acetate, propandiol butyl ether high-temperature roller are smelt coating top layer, then graphite, silica, mica sheet, alumina mixture are formed by plated film top layer by vaccum ion coater, obtains the DLC film material that radiates.The radiating DLC film material being prepared, its manufacture craft is simple, good heat dissipation effect, current temperature etc. is changed sensitive, has preferable application prospect.
Description
Technical field
The present invention relates to thin-film material technical field, is related specifically to a kind of preparation side for the DLC film material that radiates
Method.
Background technology
The forbidden band of diamond thin is wide, and resistivity and thermal conductivity are big, and carrier mobility is high, and dielectric constant is small, breakdown potential
Pressure is high, is a kind of electric thin functional material of excellent performance, and application prospect is very wide.In recent years, with science and technology development,
People have developed the preparation method of a variety of diamond thins, for example ion beam deposition, magnetron sputtering method, heat induced chemical gas phase are sunk
The such as area method, Plasma Enhanced Chemical Vapor Deposition (PECVD) have successfully been obtained the film of the speed of growth soon, with better quality, so that Buddha's warrior attendant
Stone film possesses the possibility of business application.Diamond thin belongs to cubic system, face-centered cubic structure cell, and each structure cell contains 8 C
Atom, each C atoms take 4 C atoms of sp3 hydridization and surrounding to form covalent bond, firm covalent bond and space net structure
It is that the reason for diamond hardness is very high diamond thins have many excellent properties：Hardness is high, wearability is good, coefficient of friction is imitated,
Chemical stability is high, thermal conductivity is high, thermal coefficient of expansion is small, is excellent insulator., can be direct by it using its high thermal conductivity
Product turns into the thin layer that had not only radiated but also insulated on silicon materials, is that high-frequency microwave device, super large-scale integration are optimal scattered
Hot material.It is big using its resistivity, the crystalline substance of the diode of hot operation, microwave oscillation device and high temperature high voltage resistant can be made
Body pipe and millimeter wave power device etc..
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation method for the DLC film material that radiates, the work
Skill utilizes 25%H2O2Film-substrate is handled, by nickel powder, ethyl acetate, tetrahydrofuran, pentyl acetate, propandiol butyl ether high temperature roll milling
Into coating top layer, graphite, silica, mica sheet, alumina mixture are then formed by plated film by vaccum ion coater
Top layer, obtain the DLC film material that radiates.The radiating DLC film material being prepared, its manufacture craft is simple,
Good heat dissipation effect, to current temperature etc. change it is sensitive, there is preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method for the DLC film material that radiates, comprises the following steps：
（1）Film-substrate is cleaned, utilizes 25%H2O2Washing three times, after naturally dry, is placed in argon gas atmosphere, simultaneously
Top layer is sprayed with high-temperature acidic steam, handles 10-20min；
（2）1 part of nickel powder, 3 parts of ethyl acetate, 5 parts of tetrahydrofuran, 2 parts of pentyl acetate, 5 parts of propandiol butyl ether are mixed and added instead
Kettle is answered, 300-500 DEG C of roll milling 2h, 1 part of PPG, 1 part of expoxy propane is then added, 220- is cooled to after stirring
250 DEG C of insulations are standby；
（3）By step（2）Mixed liquor be coated in step（1）The film-substrate top layer of processing, then carries out heat treatment drying, obtains
To thin-film material early-products；
（4）Graphite, silica, mica sheet, aluminum oxide etc. are according to mass ratio 12:8:7:3 mixing, are placed in high speed ball mill
Row grinding dispersion；
（5）By step（4）Mixture of powders injection vaccum ion coater in, to step（3）Thin-film material early-products enter
Row plated film, gets product.
Preferably, the step（1）In high-temperature acidic vapor (steam) temperature be 650-700 DEG C, the nitre containing 7% hydrochloric acid and 3.5%
Aqueous acid mixture.
Preferably, the step（3）In the dry parameter of heat treatment to pass through 360 DEG C, 5-10sec, 180 DEG C successively,
10-20sec, 95 DEG C, 20-30sec, finally in 65 DEG C of heat preservation and drynesses.
Preferably, the step（4）In high speed ball mill parameter be ratio of grinding media to material 99:5, speed is 1500 revs/min.
Preferably, the step（5）In the parameter of vaccum ion coater be vacuum 2.5*10-2-4.0*10-3Pa, argon
Gas atmosphere, voltage 2-3KV.
Compared with prior art, its advantage is the present invention：
（1）The preparation method of the radiating DLC film material of the present invention utilizes 25%H2O2Handle film-substrate, by nickel powder,
Ethyl acetate, tetrahydrofuran, pentyl acetate, propandiol butyl ether high-temperature roller are smelt coating top layer, then pass through vacuum ion membrane plating
Graphite, silica, mica sheet, alumina mixture are formed plated film top layer by machine, obtain the DLC film material that radiates.System
The standby radiating DLC film material formed, its manufacture craft is simple, good heat dissipation effect, current temperature etc. is changed it is sensitive,
With preferable application prospect.
（2）The radiating DLC film material feedstock of the present invention is easy to get, technique is simple, is transported suitable for heavy industrialization
With practical.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
（1）Film-substrate is cleaned, utilizes 25%H2O2Washing three times, after naturally dry, is placed in argon gas atmosphere, simultaneously
Top layer is sprayed with high-temperature acidic steam, high-temperature acidic vapor (steam) temperature is 650 DEG C, containing 7% hydrochloric acid and the mixing of 3.5% aqueous solution of nitric acid
Thing, handle 10min；
（2）1 part of nickel powder, 3 parts of ethyl acetate, 5 parts of tetrahydrofuran, 2 parts of pentyl acetate, 5 parts of propandiol butyl ether are mixed and added instead
Kettle is answered, 300 DEG C of roll milling 2h, 1 part of PPG, 1 part of expoxy propane is then added, 220 DEG C of insulations is cooled to after stirring
It is standby；
（3）By step（2）Mixed liquor be coated in step（1）The film-substrate top layer of processing, then carries out heat treatment drying, its
The dry parameter of middle heat treatment is passes through 360 DEG C, 5sec, 180 DEG C, 10sec, 95 DEG C, 20sec successively, finally in 65 DEG C of insulations
Dry, obtain thin-film material early-products；
（4）Graphite, silica, mica sheet, aluminum oxide etc. are according to mass ratio 12:8:7:3 mixing, are placed in high speed ball mill
Row grinding dispersion, fast ball mill parameter are ratio of grinding media to material 99:5, speed is 1500 revs/min；
（5）By step（4）Mixture of powders injection vaccum ion coater in, to step（3）Thin-film material early-products enter
Row plated film, the parameter of vaccum ion coater is vacuum 2.5*10-2Pa, argon gas atmosphere, voltage 2KV, get product.
The performance test results of obtained radiating DLC film material are as shown in table 1.
Embodiment 2
（1）Film-substrate is cleaned, utilizes 25%H2O2Washing three times, after naturally dry, is placed in argon gas atmosphere, simultaneously
Top layer is sprayed with high-temperature acidic steam, high-temperature acidic vapor (steam) temperature is 700 DEG C, containing 7% hydrochloric acid and the mixing of 3.5% aqueous solution of nitric acid
Thing, handle 20min；
（2）1 part of nickel powder, 3 parts of ethyl acetate, 5 parts of tetrahydrofuran, 2 parts of pentyl acetate, 5 parts of propandiol butyl ether are mixed and added instead
Kettle is answered, 500 DEG C of roll milling 2h, 1 part of PPG, 1 part of expoxy propane is then added, 250 DEG C of insulations is cooled to after stirring
It is standby；
（3）By step（2）Mixed liquor be coated in step（1）The film-substrate top layer of processing, then carries out heat treatment drying, its
The dry parameter of middle heat treatment is passes through 360 DEG C, 10sec, 180 DEG C, 20sec, 95 DEG C, 30sec successively, finally in 65 DEG C of insulations
Dry, obtain thin-film material early-products；
（4）Graphite, silica, mica sheet, aluminum oxide etc. are according to mass ratio 12:8:7:3 mixing, are placed in high speed ball mill
Row grinding dispersion, fast ball mill parameter are ratio of grinding media to material 99:5, speed is 1500 revs/min；
（5）By step（4）Mixture of powders injection vaccum ion coater in, to step（3）Thin-film material early-products enter
Row plated film, the parameter of vaccum ion coater is vacuum 4.0*10-3Pa, argon gas atmosphere, voltage 3KV, get product.
The performance test results of obtained radiating DLC film material are as shown in table 1.
Comparative example 1
（1）Film-substrate is cleaned, utilizes 25%H2O2Washing three times, naturally dry；
（2）3 parts of ethyl acetate, 5 parts of tetrahydrofuran, 2 parts of pentyl acetate, 5 parts of propandiol butyl ether are mixed and add reactor, 500
DEG C roll milling 2h, 1 part of PPG, 1 part of expoxy propane are then added, it is standby that 220 DEG C of insulations are cooled to after stirring；
（3）By step（2）Mixed liquor be coated in step（1）The film-substrate top layer of processing, then carries out heat treatment drying, its
The dry parameter of middle heat treatment is passes through 360 DEG C, 10sec, 180 DEG C, 20sec, 95 DEG C, 30sec successively, finally in 65 DEG C of insulations
Dry, obtain thin-film material early-products；
（4）Graphite, silica, mica sheet, aluminum oxide etc. are according to mass ratio 12:8:7:3 mixing, are placed in high speed ball mill
Row grinding dispersion, fast ball mill parameter are ratio of grinding media to material 99:5, speed is 1500 revs/min；
（5）By step（4）Mixture of powders injection vaccum ion coater in, to step（3）Thin-film material early-products enter
Row plated film, the parameter of vaccum ion coater is vacuum 4.0*10-3Pa, argon gas atmosphere, voltage 3KV, get product.
The performance test results of obtained radiating DLC film material are as shown in table 1.
By the obtained radiating DLC film material and commercially available common similar thin-film material of embodiment 1-2 and comparative example
This several thermal conductivity factor, density of photocurrent, dielectric constant performance tests are carried out respectively.
Table 1
| Thermal conductivity factor（W/mK） | Density of photocurrent mA/cm | Dielectric constant（εr） | |
| Embodiment 1 | 12.3 | 1.31 | 11618 |
| Embodiment 2 | 11.7 | 1.35 | 11467 |
| Comparative example 1 | 3.4 | 1.11 | 10782 |
| Commercially available film | 2.8 | 1.21 | 3494 |
The preparation method of the radiating DLC film material of the present invention utilizes 25%H2O2Film-substrate is handled, by nickel powder, acetic acid
Ethyl ester, tetrahydrofuran, pentyl acetate, propandiol butyl ether high-temperature roller are smelt coating top layer, then will by vaccum ion coater
Graphite, silica, mica sheet, alumina mixture form plated film top layer, obtain the DLC film material that radiates.Prepare and
Into radiating DLC film material, its manufacture craft is simple, good heat dissipation effect, current temperature etc. is changed sensitive, has
Preferable application prospect.The radiating DLC film material feedstock of the present invention is easy to get, technique is simple, suitable for heavy industrialization
With practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method for the DLC film material that radiates, it is characterised in that comprise the following steps：
（1）Film-substrate is cleaned, utilizes 25%H2O2Washing three times, after naturally dry, is placed in argon gas atmosphere, uses simultaneously
High-temperature acidic steam sprays top layer, handles 10-20min；
（2）1 part of nickel powder, 3 parts of ethyl acetate, 5 parts of tetrahydrofuran, 2 parts of pentyl acetate, 5 parts of propandiol butyl ether are mixed and added instead
Kettle is answered, 300-500 DEG C of roll milling 2h, 1 part of PPG, 1 part of expoxy propane is then added, 220- is cooled to after stirring
250 DEG C of insulations are standby；
（3）By step（2）Mixed liquor be coated in step（1）The film-substrate top layer of processing, then carries out heat treatment drying, obtains
To thin-film material early-products；
（4）Graphite, silica, mica sheet, aluminum oxide etc. are according to mass ratio 12:8:7:3 mixing, are placed in high speed ball mill
Row grinding dispersion；
（5）By step（4）Mixture of powders injection vaccum ion coater in, to step（3）Thin-film material early-products enter
Row plated film, gets product.
A kind of 2. preparation method of DLC film material that radiates according to claim 1, it is characterised in that the step
Suddenly（1）In high-temperature acidic vapor (steam) temperature be 650-700 DEG C, the aqueous solution of nitric acid mixture containing 7% hydrochloric acid and 3.5%.
A kind of 3. preparation method of DLC film material that radiates according to claim 1, it is characterised in that the step
Suddenly（3）In the dry parameter of heat treatment to pass through 360 DEG C, 5-10sec, 180 DEG C, 10-20sec, 95 DEG C successively, 20-
30sec, finally in 65 DEG C of heat preservation and drynesses.
A kind of 4. preparation method of DLC film material that radiates according to claim 1, it is characterised in that the step
Suddenly（4）In high speed ball mill parameter be ratio of grinding media to material 99:5, speed is 1500 revs/min.
A kind of 5. preparation method of DLC film material that radiates according to claim 1, it is characterised in that the step
Suddenly（5）In the parameter of vaccum ion coater be vacuum 2.5*10-2-4.0*10-3Pa, argon gas atmosphere, voltage 2-3KV.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710784628.9A CN107604325A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method for the DLC film material that radiates |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710784628.9A CN107604325A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method for the DLC film material that radiates |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107604325A true CN107604325A (en) | 2018-01-19 |
Family
ID=61057339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710784628.9A Pending CN107604325A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method for the DLC film material that radiates |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107604325A (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5455081A (en) * | 1990-09-25 | 1995-10-03 | Nippon Steel Corporation | Process for coating diamond-like carbon film and coated thin strip |
| JPH07316818A (en) * | 1994-05-31 | 1995-12-05 | Sanyo Electric Co Ltd | Head carbon coating film covered substrate and its formation |
| JP2002187793A (en) * | 2000-10-11 | 2002-07-05 | Osg Corp | Method of smoothing diamond film and method of manufacturing diamond coated member |
| CN1492072A (en) * | 2003-06-13 | 2004-04-28 | 西安工业学院 | Surface modifying technology of diamond-like film to titanium-nickel alloy |
| CN101109064A (en) * | 2007-08-15 | 2008-01-23 | 中国航天科技集团公司第五研究院第五一○研究所 | Method of plating-manufacturing silicon doped non-hydrogen diamond membrane |
| CN101222188A (en) * | 2007-12-25 | 2008-07-16 | 哈尔滨工业大学 | Rotor or stator with gradient coating friction material |
| CN101298656A (en) * | 2008-01-18 | 2008-11-05 | 西南交通大学 | Preparation of high-hardness diamond-like multi-layer film |
| CN102130244A (en) * | 2010-12-17 | 2011-07-20 | 天津理工大学 | LED (light-emitting diode) radiating substrate based on diamond film and manufacturing method thereof |
| CN102534614A (en) * | 2011-12-30 | 2012-07-04 | 星弧涂层科技(苏州工业园区)有限公司 | Coating method for DLC (diamond-like carbon) coating on spinning reed and equipment |
| CN102605319A (en) * | 2011-01-22 | 2012-07-25 | 南京理工大学 | Method for modifying and depositing diamond-like film on surface of aluminum alloy |
| CN102983124A (en) * | 2012-11-14 | 2013-03-20 | 深圳大学 | Light emitting diode (LED) light source with cooling device |
| CN204817678U (en) * | 2015-03-25 | 2015-12-02 | 苏州涂冠镀膜科技有限公司 | Tensile mould of metal |
| CN106634128A (en) * | 2016-12-21 | 2017-05-10 | 苏州劲元油压机械有限公司 | Anti-corrosion metal coating for hydraulic cylinder and preparation method thereof |
-
2017
- 2017-09-04 CN CN201710784628.9A patent/CN107604325A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5455081A (en) * | 1990-09-25 | 1995-10-03 | Nippon Steel Corporation | Process for coating diamond-like carbon film and coated thin strip |
| JPH07316818A (en) * | 1994-05-31 | 1995-12-05 | Sanyo Electric Co Ltd | Head carbon coating film covered substrate and its formation |
| JP2002187793A (en) * | 2000-10-11 | 2002-07-05 | Osg Corp | Method of smoothing diamond film and method of manufacturing diamond coated member |
| CN1492072A (en) * | 2003-06-13 | 2004-04-28 | 西安工业学院 | Surface modifying technology of diamond-like film to titanium-nickel alloy |
| CN101109064A (en) * | 2007-08-15 | 2008-01-23 | 中国航天科技集团公司第五研究院第五一○研究所 | Method of plating-manufacturing silicon doped non-hydrogen diamond membrane |
| CN101222188A (en) * | 2007-12-25 | 2008-07-16 | 哈尔滨工业大学 | Rotor or stator with gradient coating friction material |
| CN101298656A (en) * | 2008-01-18 | 2008-11-05 | 西南交通大学 | Preparation of high-hardness diamond-like multi-layer film |
| CN102130244A (en) * | 2010-12-17 | 2011-07-20 | 天津理工大学 | LED (light-emitting diode) radiating substrate based on diamond film and manufacturing method thereof |
| CN102605319A (en) * | 2011-01-22 | 2012-07-25 | 南京理工大学 | Method for modifying and depositing diamond-like film on surface of aluminum alloy |
| CN102534614A (en) * | 2011-12-30 | 2012-07-04 | 星弧涂层科技(苏州工业园区)有限公司 | Coating method for DLC (diamond-like carbon) coating on spinning reed and equipment |
| CN102983124A (en) * | 2012-11-14 | 2013-03-20 | 深圳大学 | Light emitting diode (LED) light source with cooling device |
| CN204817678U (en) * | 2015-03-25 | 2015-12-02 | 苏州涂冠镀膜科技有限公司 | Tensile mould of metal |
| CN106634128A (en) * | 2016-12-21 | 2017-05-10 | 苏州劲元油压机械有限公司 | Anti-corrosion metal coating for hydraulic cylinder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 申勇峰编著: "《工程设备设计基础》", 28 February 2014 * |
| 苏家齐主编: "《塑料工业辞典》", 31 December 1989 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106517171B (en) | A kind of preparation method of graphene aerogel | |
| TWI607810B (en) | Process for producing semiconductive indium oxide layers, indium oxide layers prepared by the process and use thereof | |
| Reddy et al. | Investigations on SnS films deposited by spray pyrolysis | |
| CN103570014B (en) | A kind of Graphene/boron nitride stratified composite and preparation method thereof | |
| US20160281221A1 (en) | Formation method of hexagonal boron nitride thick film on a substrate and hexagonal boron nitride thick film laminates thereby | |
| CN106356638A (en) | Absorption-rate-adjustable bandwidth electromagnetic wave absorber based on graphene film | |
| CN106046409B (en) | A method of preparing surface patina Kapton | |
| CN109005607A (en) | A kind of graphene Electric radiant Heating Film and its preparation method and application and the equipment containing graphene Electric radiant Heating Film | |
| CN109709160A (en) | A kind of electron conducting metal organic frame film and its preparation method and application | |
| CN101820018A (en) | Preparation method of CdS thin-film | |
| TWI295072B (en) | Plasma cvd apparatus | |
| CN107124778A (en) | Far-infrared electrothermal film, the manufacture craft of far-infrared electrothermal film and electric heater | |
| CN107887514A (en) | A kind of preparation method and applications of perovskite thin film | |
| CN108615815A (en) | NiO bases compacted zone, perovskite solar cell and preparation method thereof | |
| CN107604325A (en) | A kind of preparation method for the DLC film material that radiates | |
| CN103801354B (en) | A kind of graphite phase carbon nitride hollow ball visible light catalyst of after annealing process | |
| CN106011786B (en) | Atmospheric pressure disperse electric discharge device and metal surface deposition class SiO2Film process | |
| CN109957784A (en) | A kind of prepared by microwave plasma chemical vapor deposition prepares silica/graphene nanocomposite material method and products thereof | |
| CN104716222B (en) | The method that radio frequency cracks selenium steam production CIGS thin-film | |
| CN112851334A (en) | Heating body based on silicon nitride and preparation process thereof | |
| CN103241730A (en) | Method for doping patterned atoms on surface of graphene by using molecular template | |
| CN108190868A (en) | A kind of preparation method of grapheme material | |
| CN114573330A (en) | Defective graphene/wave-transparent ceramic composite wave-absorbing material, method and application | |
| CN107698171A (en) | A kind of preparation method of TiN coated glasses | |
| CN110150940A (en) | A kind of graphene-based environmental protection carpet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180119 |