CN103160776A - Titanium diboride-nickel coating or film and preparation method thereof - Google Patents
Titanium diboride-nickel coating or film and preparation method thereof Download PDFInfo
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- CN103160776A CN103160776A CN2011104189288A CN201110418928A CN103160776A CN 103160776 A CN103160776 A CN 103160776A CN 2011104189288 A CN2011104189288 A CN 2011104189288A CN 201110418928 A CN201110418928 A CN 201110418928A CN 103160776 A CN103160776 A CN 103160776A
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Abstract
The invention relates to a titanium diboride-nickel coating or film and a preparation method thereof. The coating or film is characterized by being prepared from a main phase TiB2 and a secondary crystalline phase metal Ni by using a physical vapor deposition technique for in situ synthesis; the TiB2 accounts for 65 95at.%, and the Ni accounts for of is 5 - 35at.%; and a substrate of the coating or film is made of monocrystal silicon, glass, high speed steel, alloy steel or titanium alloy; and the film has thickness of 20 nm-1um, and the coating has thickness of 1um-1mm. he invention designs a novel coating material system namely a metal Ni toughened TiB2 coating or film prepared through in-situ synthesis; and the coating has hardness up to higher than 25GPa, good conductive properties, good toughness, corrosion resistance and erosion resistance, and excellent friction and wear performance, and can be widely applied to the fields of cutting tool, mold, electric contact and protection. The preparation process has advantages of simpleness, short production cycle and low cost, and is convenient for industrialized mass production.
Description
Technical field
The invention belongs to field of new, relate to a kind of TiB
2-Ni material is specifically related to the synthetic toughness reinforcing TiB of metal Ni of a kind of original position
2Coating or film and preparation method thereof.
Background technology
TiB
2Have the advantages such as high rigidity, high-melting-point, low density, higher Young's modulus, good heat conduction, conduction, wear-resisting and chemical stability, it is a kind of advanced ceramics material with good structure and function performance, therefore it is widely used in multiple fields, the coated material such as particularly can be used as hard, protect, electrically contact.Yet TiB
2The fragility of stupalith has limited its independent application to a certain extent, therefore, uses for reference the Research Thinking of Material cladding, based on TiB
2The high rigidity of material, TiB
2The metal-base composites that particle strengthens is widely studied recently.For example: titanium diboride dispersed and strengthened copper-based composite material (Chinese patent, 200910095176.9), TiB
2Particle reinforced magnesium base compound material (Chinese patent, 200710047943.X) etc., these materials have well kept the premium propertiess such as the toughness, electroconductibility, workability of metallic matrix, have improved to a certain extent again intensity and the hardness of metal, have good application prospect.Yet, the TiB in material
2Just as wild phase a small amount of make an addition to metallic matrix inside, this improvement to the strength of materials and hardness is extremely limited.Otherwise, with TiB
2In addition the report of the compound material of a small amount of metallographic phase is actually rare for principal crystalline phase.The TiB that Zhang Xinghong etc. will obtain in advance
2Phase and metallographic phase have obtained TiB by techniques such as sintering
2Content Gao Deda 75% and the lower block composite material of Cu-Ni content, prepared material is near equilibrium state.(Xinghong Zhang, Changqing Hong, Jiecai Hana and Hexin Zhang, Microstructure and mechanical properties of TiB
2/ (Cu, Ni) interpenetrating phase composites, Scripta Materialia, 55,2006,565-568) and the synthetic toughness reinforcing TiB of metal Ni of original position gas phase
2Coating or film do not appear in the newspapers.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind ofly not only has high rigidity but also have good toughness, and friction resistant, polishing machine, conductivity and resistance to chemical corrosion all show good TiB simultaneously
2-Ni coating or film.
Second technical problem to be solved by this invention is to provide a kind of TiB
2-Ni coating or thin film technology method, not only preparation cost is low, and simple to operate, preparation cycle is short, repeatability is strong, can be used for large-scale commercial production.
The present invention solves the technical scheme that above-mentioned first technical problem adopts: a kind of TiB
2-Ni coating or film is characterized in that this TiB
2-Ni coating or film are with TiB
2Be principal crystalline phase, metal Ni is that paracrystalline phase utilizes the physical gas phase deposition technology original position to be composited, wherein TiB
2Content is 65-95at.%, and Ni content is 5-35at.%.
As preferably, described TiB
2The baseplate material of-Ni coating or film is selected silicon single crystal, glass, rapid steel, steel alloy or titanium alloy etc.
At last, the thickness of described film is 20nm-1um; The thickness of described coating is 1um-1mm.
The present invention solves the technical scheme that above-mentioned second technical problem adopt: a kind of above-mentioned TiB
2-Ni coating or thin film technology method is characterized in that with highly purified TiB
2Ceramic target and metal Ni target are raw material, adopt physical gas phase deposition technology, by in-situ deposition different Ti B
2With coating or the film of Ni proportioning, as preferably, the concrete steps that magnetron sputtering technique prepares this coating or film are:
A) target and substrate are installed;
B) vacuumize and base plate heating;
C) pass into rare gas element, power supply and substrate parameter are set, build-up of luminance, after pre-sputtering, sputtering sedimentation;
D) deposition finishes, and closes electricity, gas, water route, sampling.
As improvement, described step substrate a) will be used respectively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning 10～20min successively before installation, then in 70～90 ℃ of lower forced air drying 1～2h.
Vacuumizing as preferably, described step b) refers to that in the sediment chamber, the back end vacuum is lower than 9.5 * 10
-4Pa, described base plate heating temperature is room temperature～500 ℃, insulation 20～30min.
Described step c) power supply in and substrate parameter are: TiB
2The ceramic target power parameter is: intermediate frequency 50-200KHZ, power 100-500W, dutycycle 60-90%; Ni metallic target power parameter is: dc power 0-20W; The pre-sputtering time is 8～15min, and the described sputtering sedimentation time is 30～200min.The substrate parameter is: bias voltage 0V, temperature room temperature～500 ℃.
Preferred again, described step c) rare gas element that passes in is argon gas, and inert gas flow is controlled at 20-40sccm, and with the scope of sediment chamber's internal gas pressure modulation 0.1-1Pa.
At last, described physical gas phase deposition technology is not limited to magnetron sputtering plating, also comprises other physical gas phase deposition technologies such as vacuum evaporation or ion beam assisted depositing.
Compared with prior art, the invention has the advantages that:
1) designed a kind of new coating material system, i.e. the synthetic toughness reinforcing TiB of metal Ni of original position
2Coating or film.
2) this coating hardness is up to more than 25GPa, and conductivity is good, has simultaneously good toughness and anticorrosive, Burning corrosion resistance energy and excellent friction, polishing machine.
3) preparation TiB
2The technique of-Ni coating or film is simple, and is easy to operate, and preparation cycle is short, and cost is low, is convenient to suitability for industrialized production.
Description of drawings
Fig. 1 is that the present invention prepares TiB
2-Ni coating specimen surface (XRD) collection of illustrative plates, wherein X-coordinate is diffraction angle 2 θ, and unit is °, and ordinate zou is diffraction peak intensity, and unit is a.u.;
Fig. 2 the present invention prepares TiB
2Scanning electron microscope (SEM) photo of-Ni coating sample, wherein a is section, b is the surface.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1:
1) select the TiB of commercially available purity 99.9%
2The metal Ni target of ceramic target and commercially available purity 99.99% is raw material; Substrate is selected the monocrystalline silicon substrate of (100) orientation.
2) at first carry out the cleaning of substrate, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 20min, then in 80 ℃ of lower forced air drying 2h, standby.
3) magnetic control sputtering system that adopts this seminar autonomous design to produce, at first begin to speak after correct installation base plate and target, check that first gas, electricity, water route are all normal, then open general supply, start mechanical pump, when sediment chamber and sample chamber air pressure all be in 10Pa once after, close the valve between mechanical pump and chamber, open flapper valve, start molecular pump, the slide valve of outwarding winding, vacuum reaches 10 in the sample chamber
-3After Pa, stop carefully taking out its vacuum, to accelerate the extraction speed of vacuum in the sediment chamber.
4) the back end vacuum reaches 8.7 * 10 in the sediment chamber
-5During Pa, open the sample substrate heating mode, set temperature is 200 ℃, is incubated 20min after the arrival assigned temperature, treats that vacuum tightness is evacuated to 9.1 * 10
-5Record back end vacuum tightness during Pa.
5) open argon bottle, flow control is at 30sccm, and the corresponding valve of outwarding winding passes into rare gas element, suitably closes the slide valve between sediment chamber and molecular pump, with sediment chamber's internal gas pressure modulation 0.5Pa.
6) TiB is set
2The ceramic target power parameter is: intermediate frequency (MF) 100HKZ, power 400W, dutycycle 80%; Ni metallic target power parameter is: direct current (DC), power 4W; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 180min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain final product TiB
2-Ni coating sample.
TiB with preparation
2-Ni coating typical sample carries out analytical test, obtains following result and data.TiB with gained
2The Alpha-Step IQ type surface profiler testing coating thickness that-Ni coating sample weeds scientific and technological Engineering Co., Ltd product with U.S.'s suffering is about 1.3 μ m.TiB with gained
2The surperficial crystalline phase of D8Advance type x-ray diffractometer analytic sample that the German Brooker of-Ni coating sample employing company produces forms, visible prepared TiB
2TiB in-Ni coating
2Diffraction peak strong (150a.u.), and the diffraction peak of Ni not obvious (Fig. 1).Adopt the S-4800 type surface sweeping electron microscope of HIT's production to prepared TiB
2-Ni coating sample carries out surface and section microstructure analysis, can find out that from the Photomicrograph (Fig. 2) of coatingsurface this coatingsurface is more smooth, fine and close and do not have tiny crack to produce; Can find obviously that from the section Photomicrograph of coating this coat-thickness homogeneous, crystal are columnar growth, arrange closely.TiB to gained
2The AXIS UTLTRADLD type XPS that the Japanese Shimadzu of-Ni coating sample employing company produces analyzes, and shows that the inner Ni content of coating is probably 20.50%.With prepared TiB
2-Ni coating sample records coating under the upper 5N power of multifunction friction wear trier (UMT-3) frictional coefficient is about 0.68, and the sample wearing and tearing had no inefficacy after 1 hour, visible TiB
2-Ni coating has good wear Characteristics.At last with prepared TiB
2-Ni coating sample carries out the acid-fast alkali-proof corrosion at normal temperatures, and result shows that coating has good stability.
Embodiment 2:
1) select the TiB of commercially available purity 99.9%
2The metal Ni target of ceramic target and commercially available purity 99.99% is raw material; Substrate is selected the ordinary plate glass substrate.
2) at first carry out the cleaning of substrate, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 20min, then in 80 ℃ of lower forced air drying 2h, standby.
3) magnetic control sputtering system that adopts this seminar autonomous design to produce, at first begin to speak after correct installation base plate and target, check that first gas, electricity, water route are all normal, then open general supply, start mechanical pump, when sediment chamber and sample chamber air pressure all be in 10Pa once after, close the valve between mechanical pump and chamber, open flapper valve, start molecular pump, the slide valve of outwarding winding, vacuum reaches 10 in the sample chamber
-3After Pa, stop carefully taking out its vacuum, to accelerate the extraction speed of vacuum in the sediment chamber.
4) the back end vacuum reaches 7 * 10 in the sediment chamber
-5During Pa, open the sample substrate heating mode, set temperature is 300 ℃, is incubated 20min after the arrival assigned temperature, treats that vacuum tightness is evacuated to 7.8 * 10
-5Record back end vacuum tightness during Pa.
5) open argon bottle, flow control is at 26sccm, and the corresponding valve of outwarding winding passes into rare gas element, suitably closes the slide valve between sediment chamber and molecular pump, with sediment chamber's internal gas pressure modulation 0.3Pa.
6) TiB is set
2The ceramic target power parameter is: intermediate frequency (MF) 150HKZ, power 300W, dutycycle 90%; Ni metallic target power parameter is: direct current (DC), power 8W; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 30min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain final product TiB
2-Ni film sample.
Embodiment 3:
1) select the TiB of commercially available purity 99.9%
2The metal Ni target of ceramic target and commercially available purity 99.99% is raw material; Substrate is selected the rapid steel substrate.
2) at first carry out the cleaning of substrate, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 20min, then in 80 ℃ of lower forced air drying 2h, standby.
3) magnetic control sputtering system that adopts this seminar autonomous design to produce, at first begin to speak after correct installation base plate and target, check that first gas, electricity, water route are all normal, then open general supply, start mechanical pump, when sediment chamber and sample chamber air pressure all be in 10Pa once after, close the valve between mechanical pump and chamber, open flapper valve, start molecular pump, the slide valve of outwarding winding, vacuum reaches 10 in the sample chamber
-3After Pa, stop carefully taking out its vacuum, to accelerate the extraction speed of vacuum in the sediment chamber.
4) the back end vacuum reaches 5 * 10 in the sediment chamber
-5During Pa, open the sample substrate heating mode, set temperature is 500 ℃, is incubated 30min after the arrival assigned temperature, treats that vacuum tightness is evacuated to 5.8 * 10
-5Record back end vacuum tightness during Pa.
5) open argon bottle, flow control is at 20sccm, and the corresponding valve of outwarding winding passes into rare gas element, suitably closes the slide valve between sediment chamber and molecular pump, with sediment chamber's internal gas pressure modulation 0.2Pa.
6) TiB is set
2The ceramic target power parameter is: intermediate frequency (MF) 50HKZ, power 400W, dutycycle 70%; Ni metallic target power parameter is: direct current (DC), power 18W; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 40min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain final product TiB
2-Ni coating sample.
Embodiment 4:
1) select the TiB of commercially available purity 99.9%
2The metal Ni target of ceramic target and commercially available purity 99.99% is raw material; Substrate is selected titanium alloy substrate.
2) at first carry out the cleaning of substrate, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 15min, then in 80 ℃ of lower forced air drying 1h, standby.
3) magnetic control sputtering system that adopts this seminar autonomous design to produce, at first begin to speak after correct mounting plate and target, check that first gas, electricity, water route are all normal, then open general supply, start mechanical pump, when sediment chamber and sample chamber air pressure all be in 10Pa once after, close the valve between mechanical pump and chamber, open flapper valve, start molecular pump, the slide valve of outwarding winding, vacuum reaches 10 in the sample chamber
-3After Pa, stop carefully taking out its vacuum, to accelerate the extraction speed of vacuum in the sediment chamber.
4) the back end vacuum reaches 8 * 10 in the sediment chamber
-5During Pa, record back end vacuum tightness.
5) open argon bottle, flow control is at 35sccm, and the corresponding valve of outwarding winding passes into rare gas element, suitably closes the slide valve between sediment chamber and molecular pump, with sediment chamber's internal gas pressure modulation 0.8Pa.
6) TiB is set
2The ceramic target power parameter is: intermediate frequency (MF) 100HKZ, power 200W, dutycycle 80%; Ni metallic target power parameter is: direct current (DC), power 15W; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 180min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain final product TiB
2-Ni coating sample.
Claims (9)
1. a TiB2-nickel coating or film, is characterized in that this TiB
2-Ni coating or film are with TiB
2Be principal crystalline phase, metal Ni is compound coating or the thin-film material that paracrystalline phase utilizes the physical gas phase deposition technology original position to be composited, wherein TiB
2Content is 65-95at.%, and Ni content is 5-35at.%.
2. TiB2-nickel coating according to claim 1 or film, is characterized in that described TiB
2The baseplate material of-Ni coating or film is selected silicon single crystal, glass, rapid steel, steel alloy or titanium alloy etc.
3. TiB2-nickel coating according to claim 1 or film, the thickness that it is characterized in that described film is 20nm-1um; The thickness of described coating is 1um-1mm.
4. a described TiB2-nickel coating or thin film technology method, is characterized in that with TiB
2Ceramic target and metal Ni target are raw material, adopt physical gas phase deposition technology, in-situ deposition different Ti B
2With coating or the film of Ni proportioning, concrete steps are:
A) target and substrate are installed;
B) vacuumize and base plate heating;
C) pass into rare gas element, power supply and substrate parameter are set, build-up of luminance, after pre-sputtering, sputtering sedimentation;
D) deposition finishes, and closes electricity, gas, water route, sampling.
5. preparation method according to claim 4 is characterized in that described step substrate a) will use respectively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning 10～20min successively before installation, then in 70～90 ℃ of lower forced air drying 1～2h.
6. preparation method according to claim 4, is characterized in that described step b) in vacuumize and refer to that in the sediment chamber, the back end vacuum is lower than 9.5 * 10
-4Pa, described base plate heating temperature is room temperature～500 ℃, insulation 20～30min.
7. preparation method according to claim 4, is characterized in that described step c) in power supply and substrate parameter be: TiB2 ceramic target power parameter is: intermediate frequency 50-200KHZ, power 100-500W, dutycycle 60-90%; Ni metallic target power parameter is: dc power 0-20W; The pre-sputtering time is 8～15min, and the described sputtering sedimentation time is 30～200min; The substrate parameter is bias voltage 0V, temperature room temperature～500 ℃.
8. preparation method according to claim 4, is characterized in that described step c) in the rare gas element that passes into be argon gas, inert gas flow is controlled at 20-40sccm, and with the scope of sediment chamber's internal gas pressure modulation 0.1-1Pa.
9. preparation method according to claim 4, is characterized in that described physical gas phase deposition technology is not limited to magnetron sputtering plating, also comprises vacuum evaporation or ion beam assisted depositing.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451648A (en) * | 2013-09-02 | 2013-12-18 | 山东大学 | Laser clad TiB2-Ni based metal ceramic coating and preparation method thereof |
| CN103849834A (en) * | 2014-02-20 | 2014-06-11 | 西工大常熟研究院有限公司 | Compound cutting tool coating based on titanium diboride and preparation method thereof |
| CN105271280A (en) * | 2014-06-27 | 2016-01-27 | 三星电子株式会社 | Electrically conductive thin films and electronic device comprising the same |
| CN107012424A (en) * | 2017-03-10 | 2017-08-04 | 广东工业大学 | A kind of TiZrB2Hard coat and its preparation method and application |
| CN107338418A (en) * | 2017-08-30 | 2017-11-10 | 深圳先进技术研究院 | Transition metal boride metal composite target, filming equipment and application thereof |
| CN110729445A (en) * | 2018-07-16 | 2020-01-24 | 深圳先进技术研究院 | Tab with coating, preparation method thereof, battery cell, battery and electric tool |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451648A (en) * | 2013-09-02 | 2013-12-18 | 山东大学 | Laser clad TiB2-Ni based metal ceramic coating and preparation method thereof |
| CN103451648B (en) * | 2013-09-02 | 2016-05-04 | 山东大学 | A kind of laser melting coating TiB2-Ni based metal ceramic coating and preparation method thereof |
| CN103849834A (en) * | 2014-02-20 | 2014-06-11 | 西工大常熟研究院有限公司 | Compound cutting tool coating based on titanium diboride and preparation method thereof |
| CN105271280A (en) * | 2014-06-27 | 2016-01-27 | 三星电子株式会社 | Electrically conductive thin films and electronic device comprising the same |
| CN107012424A (en) * | 2017-03-10 | 2017-08-04 | 广东工业大学 | A kind of TiZrB2Hard coat and its preparation method and application |
| CN107012424B (en) * | 2017-03-10 | 2020-09-08 | 广东工业大学 | TiZrB2Hard coating and preparation method and application thereof |
| CN107338418A (en) * | 2017-08-30 | 2017-11-10 | 深圳先进技术研究院 | Transition metal boride metal composite target, filming equipment and application thereof |
| CN110729445A (en) * | 2018-07-16 | 2020-01-24 | 深圳先进技术研究院 | Tab with coating, preparation method thereof, battery cell, battery and electric tool |
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