CN103160777A - Titanium diboride-nickel thin film with coating structure and preparation method thereof - Google Patents
Titanium diboride-nickel thin film with coating structure and preparation method thereof Download PDFInfo
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- CN103160777A CN103160777A CN2011104189767A CN201110418976A CN103160777A CN 103160777 A CN103160777 A CN 103160777A CN 2011104189767 A CN2011104189767 A CN 2011104189767A CN 201110418976 A CN201110418976 A CN 201110418976A CN 103160777 A CN103160777 A CN 103160777A
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Abstract
The invention relates to a titanium diboride-nickel thin film with coating structure. The TiB2-Ni thin film is characterized by being prepared from a continuous phase metal Ni and a dispersed phase TiB2 grains through in-situ synthesis. In the TiB2-Ni thin film, metal Ni in a three-dimensional continuous cellular structure uniformly form a basic framework of the thin film, and the TiB2 grains in granular shape uniformly fill in the cellular structure, so as to form a coating microstructure with metal Ni evenly coated with TiB2 grains; and the TiB2 accounts for 60- 95at.%, and Ni accounts for 5-40at.%. The TiB2-Ni thin film with coating structure provided by the invention shows good toughness and high hardness, so as to greatly expand the scope of application of the thin film. A double-target co-sputtering magnetron sputtering technology is easy to operate; composition, structure and performance of the TiB2-Ni thin film material can be well controlled through control of process conditions; and the method does not require a post-treatment process, has short preparation period, low cost and good reproducibility, and is easy to realize industrialized production.
Description
Technical field
The invention belongs to field of new, relate to a kind of TiB
2-Ni film, specifically a kind of TiB of clad structure
2-Ni film and preparation method thereof.
Background technology
TiB
2Having the advantages such as high rigidity, high-melting-point, low density, higher Young's modulus, good heat conduction, conduction, wear-resisting and chemical stability, is a kind of advanced ceramics material with good structure properties and functional performance.Based on TiB
2The high rigidity of material, TiB
2The metal-base composites that particle strengthens is widely studied.For example: titanium diboride dispersed and strengthened copper-based composite material (Chinese invention patent, 200910095176.9), TiB
2Particle reinforced magnesium base compound material (Chinese invention 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 a small amount of (the common TiB of wild phase
2≤ 20at.%) be distributed in metallic matrix inside, this improvement to the strength of materials and hardness is extremely limited.
In order further to improve hardness and the intensity of metallic substance, the present invention proposes a kind of new mentality of designing, has greatly improved wild phase TiB in material
2Content be a kind of rich TiB
2The thin-film material of phase, in order better to keep the toughness of original metal Ni, the present invention has built a kind of clad structure, both a kind of nanometer Ni layer three-dimensional wrapping TiB simultaneously
2Born of the same parents' shape microstructure of particle has the TiB of this clad structure
2-Ni film there is not yet report.
Up to the present, the thin film technology method has a variety of, mainly is divided into chemical process and the large class of physical method two.Wherein physical gas phase deposition technology enters gas phase due to the source material through physical process, and under low pressure carries out, so film is combined with matrix well, be convenient to simultaneously large-scale continuous industrial production, thereby development in recent years is rapid.The present invention adopts the magnetron sputtering technique preparation the most widely of industrial applications in physical gas phase deposition technology to have the TiB of clad structure
2-Ni film.
Summary of the invention
First technical problem to be solved by this invention is to build a kind of TiB with clad structure
2-Ni film, the film of this structure had both had good toughness, had again good hardness and intensity.
Second technical problem to be solved by this invention is to provide a kind of TiB with clad structure
2-Ni thin film technology method, preparation technology is simple, and the cycle is short, and cost is low, and reproducibility is good, is convenient to realize suitability for industrialized production.
The present invention solves the technical scheme that above-mentioned first technical problem adopts: a kind of TiB with clad structure
2-Ni film is characterized in that this TiB
2-Ni film is take metal Ni as external phase, TiB
2Crystal grain is that the disperse phase original position is composited, at this TiB
2In-Ni film, metal Ni evenly consists of the basic boom of film with the continuous cell structure of three-dimensional, and TiB
2Crystal grain fills up inner at cell structure uniformly with particulate state, forms metal Ni and evenly wraps up TiB
2The coating microstructure of crystal grain, wherein TiB
2Content is 60-95at.%, and Ni content is 5-40at.%.
As preferably, described TiB
2The baseplate material of-Ni film is selected silicon single crystal, glass, rapid steel, steel alloy, titanium alloy, copper alloy or nickelalloy etc.
Described TiB
2TiB in-Ni film
2Born of the same parents' shape crystal grain is of a size of 2-80nm, and its outer evenly thickness of the metal Ni layer of parcel is 0.5-20nm.
The present invention solves the technical scheme that above-mentioned second technical problem adopt: a kind of TiB with clad structure
2-Ni thin film technology method is characterized in that with high-purity TiB
2Ceramic target and metal Ni target are raw material, adopt the two target codeposition technique of magnetic control sputtering system utilization to be prepared, and step is:
A) target, substrate are installed;
B) vacuumize and base plate heating: the back end vacuum is lower than 5 * 10
-5Pa, the Heating temperature scope of substrate is room temperature-500 ℃, and insulation 20-30min.
C) pass into rare gas element, power supply and substrate parameter are set, build-up of luminance, after pre-sputtering, sputtering sedimentation, wherein TiB
2The ceramic target power parameter is: intermediate frequency (MF) 50-200KHZ, power 100-500W, dutycycle 60-90%; Ni metallic target power parameter is: direct current (DC), power 0-20W; The substrate parameter is: bias voltage-100-0V, temperature room temperature-500 ℃; Pre-sputtering time 8~15min; Depositing time: 10-120min;
D) deposition finishes, and closes electricity, gas, water route, sampling.
As improvement, before installing, described step substrate a) needs to use successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning 10~20min, then in 70~90 ℃ of lower forced air drying 1~2h.
At last, described step c) rare gas element that passes in is preferably 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.
Compared with prior art, the invention has the advantages that:
1) constructed TiB
2A kind of new microstructure of-Ni film, the i.e. synthetic fully continuous TiB that wraps up of metal Ni of original position
2Film.
2) TiB of clad structure of the present invention
2-Ni film is different from traditional TiB
2The particulate reinforcement metal-base composites has shown good toughness and very high hardness, and this has greatly enlarged the range of application of this film.
3) the synthetic clad structure TiB of original position of the present invention
2-Ni thin film technology technology, easy to operate, need not aftertreatment technology, preparation cycle is short, and cost is low, and reproducibility is good, is convenient to suitability for industrialized production.
Description of drawings
Fig. 1 the present invention prepares TiB
2-Ni film typical sample 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
2Transmission electron microscope (TEM) photo of-Ni film typical sample;
Fig. 3 the present invention prepares TiB
2Scanning electron microscope (SEM) photo of cut after-Ni film typical sample friction testing.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1:
1) selecting commercially available purity is 99.9% TiB
2Ceramic target and commercially available purity are that 99.99% metal Ni target is raw material; Substrate is selected the monocrystalline silicon substrate of (100) orientation.
2) at first carry out the cleaning of matrix, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 15min, then in 80 ℃ of lower forced air drying 2h, standby.
3) the two target magnetic control sputtering system that adopts that this seminar autonomous design produces, at first after beginning to speak matrix and target correctly are installed, 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 3.7 * 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 4.1 * 10
-5Record back end vacuum tightness during Pa.
5) open argon bottle, flow control is at 33sccm, 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 0.4Pa.
6) TiB is set
2The ceramic target power parameter is: intermediate frequency (MF) 100HKZ, power 300W, dutycycle 80%; Ni metallic target power parameter is: direct current (DC), power 5W; The substrate parameter is: 300 ℃ of bias voltage 0V, temperature; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 20min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain the TiB that final product has clad structure
2-Ni film sample.
Embodiment 2:
1) selecting commercially available purity is 99.9% TiB
2Ceramic target and commercially available purity are that 99.99% metal Ni target is raw material; Substrate is selected the rapid steel substrate.
2) at first carry out the cleaning of matrix, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 20min, then in 80 ℃ of lower forced air drying 2h, standby.
3) the two target magnetic control sputtering system that adopts that this seminar autonomous design produces, at first after beginning to speak matrix and target correctly are installed, 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 2.9 * 10 in the sediment chamber
-5During Pa, open the sample substrate heating mode, set temperature is 100 ℃, is incubated 20min after the arrival assigned temperature, treats that vacuum tightness is evacuated to 3.4 * 10
-5Record back end vacuum tightness during Pa.
5) open argon bottle, flow control is at 23sccm, 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) 80HKZ, power 100W, dutycycle 90%; Ni metallic target power parameter is: direct current (DC), power 8W; The substrate parameter is: 100 ℃ of bias voltage-20V, temperature; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 100min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain the TiB that final product has clad structure
2-Ni film sample.
Embodiment 3:
1) selecting commercially available purity is 99.9% TiB
2Ceramic target and commercially available purity are that 99.99% metal Ni target is raw material; Matrix is selected titanium alloy substrate.
2) at first carry out the cleaning of matrix, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 10min, then in 80 ℃ of lower forced air drying 2h, standby.
3) the two target magnetic control sputtering system that adopts that this seminar autonomous design produces, at first after beginning to speak matrix and target correctly are installed, 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 2.9 * 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 3.2 * 10
-5Record back end vacuum tightness during Pa.
5) open argon bottle, flow control is at 25sccm, 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 0.9Pa.
6) TiB is set
2The ceramic target power parameter is: intermediate frequency (MF) 150HKZ, power 200W, dutycycle 70%; Ni metallic target power parameter is: direct current (DC), power 15W; The substrate parameter is: 500 ℃ of bias voltage-80V, temperature; 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 the TiB that final product has clad structure
2-Ni film sample.
Embodiment 4:
1) selecting commercially available purity is 99.9% TiB
2Ceramic target and commercially available purity are that 99.99% metal Ni target is raw material; Substrate is selected copper alloy substrate.
2) at first carry out the cleaning of matrix, use respectively successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning substrate 20min, then in 80 ℃ of lower forced air drying 2h, standby.
3) the two target magnetic control sputtering system that adopts that this seminar autonomous design produces, at first after beginning to speak matrix and target correctly are installed, 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 1.9 * 10 in the sediment chamber
-5During Pa, without base plate heating.
5) open argon bottle, flow control is at 40sccm, 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) 180HKZ, power 300W, dutycycle 90%; Ni metallic target power parameter is: direct current (DC), power 18W; The substrate parameter is: bias voltage-50V; Behind pre-sputtering 10min left and right, open the sample baffle plate, formal sputtering deposition, depositing time: 80min.
7) after deposition finishes, close successively sample baffle plate, target power supply, gas circuit etc.; After sample was cooling, sampling namely can obtain the TiB that final product has clad structure
2-Ni film sample.
TiB with above-mentioned technique preparation
2-Ni film 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 film sample weeds scientific and technological Engineering Co., Ltd product with U.S.'s suffering is the 200nm left and right.TiB with gained
2The NANOG200 type nano-hardness tester that-Ni film sample employing American MTS company produces, recording its hardness is 35GPa.TiB with gained
2D8 Advance type x-ray diffractometer (XRD) the analytic sample surface crystalline phase composition (Fig. 1) that the German Brooker of-Ni film sample employing company produces, visible prepared TiB
2TiB in-Ni coating
2Diffraction peak have obvious broadening phenomenon, can infer TiB wherein
2Crystal grain is nano level, and there is no the diffraction peak of obvious metal Ni in the XRD figure spectrum, thereby infers that Ni wherein is non-crystalline state.TiB to gained
2The AXIS ULTRADLD type x-ray photoelectron power spectrum (XPS) that the Japanese Shimadzu of-Ni film sample employing company produces is analyzed, and shows that the inner Ni content of coating is probably 17%.TiB with preparation
2Analyze (Fig. 2) under the Tecnai F20 projection electron microscope (TEM) that-Ni film sample adopts U.S. FEI Co. to produce, can obviously find out the TiB of gained
2-Ni film has typical clad structure, TiB
2Disperse phase is cell structure, and particle diameter is 5-15nm, and metal Ni evenly is wrapped in TiB
2Particle is outer, and thickness is 1-3nm, and continuous metal Ni has consisted of continuous three-dimensional network-like structure simultaneously.In order to prove prepared TiB
2-Ni film has good toughness, described film sample is carried out friction testing, and the cut sample is carried out microstructure analysis under the S-4800 type surface sweeping electron microscope (SEM) that HIT produces, the Photomicrograph of cut (Fig. 3) shows, around cut film without significantly burst apart, peeling phenomenon, the surface film material has good toughness.
Claims (6)
1. the TiB2 with clad structure-nickel film, is characterized in that this TiB
2-Ni film is take metal Ni as external phase, TiB
2Crystal grain is that the disperse phase original position is composited, at this TiB
2In-Ni film, metal Ni evenly consists of the basic boom of film with the continuous cell structure of three-dimensional, and TiB
2Crystal grain fills up inner at cell structure uniformly with particulate state, forms metal Ni and evenly wraps up TiB
2The coating microstructure of crystal grain, wherein TiB
2Content is 60-95at.%, and Ni content is 5-40at.%.
2. TiB2 according to claim 1-nickel film, is characterized in that described TiB
2The baseplate material of-Ni film is selected silicon single crystal, glass, rapid steel, steel alloy, titanium alloy, copper alloy or nickelalloy.
3. TiB2 according to claim 1-nickel film, is characterized in that described TiB
2TiB in-Ni film
2Born of the same parents' shape crystal grain is of a size of 2-80nm, and its outer evenly thickness of the metal Ni layer of parcel is 0.5-20nm.
4. described TiB2 with clad structure-nickel thin film technology method is characterized in that adopting the two target codeposition technique of magnetic control sputtering system utilization to be prepared take ceramic target and metal Ni target as raw material, and step is:
A) target, substrate are installed;
B) vacuumize and base plate heating: the back end vacuum is lower than 5 * 10
-5Pa, the Heating temperature scope of substrate is room temperature-500 ℃, and insulation 20-30min.
C) pass into rare gas element, power supply and substrate parameter are set, build-up of luminance, after pre-sputtering, sputtering sedimentation, wherein TiB
2The ceramic target power parameter is: intermediate frequency (MF) 50-200KHZ, power 100-500W, dutycycle 60-90%; Ni metallic target power parameter is: direct current (DC), power 0-20W; The substrate parameter is: bias voltage-100-0V, temperature room temperature-500 ℃; Pre-sputtering time 8~15min; Depositing time: 10-120min;
D) deposition finishes, and closes electricity, gas, water route, sampling.
5. preparation method according to claim 4, is characterized in that needing to use successively dehydrated alcohol, acetone, dehydrated alcohol ultrasonic cleaning 10~20min before described step substrate a) is installed, then in 70~90 ℃ of lower forced air drying 1~2h.
6. 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.
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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 |
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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 |
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