CN105002467B - A kind of Cu Ti amorphous alloy films and preparation method thereof - Google Patents
A kind of Cu Ti amorphous alloy films and preparation method thereof Download PDFInfo
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- CN105002467B CN105002467B CN201510509138.9A CN201510509138A CN105002467B CN 105002467 B CN105002467 B CN 105002467B CN 201510509138 A CN201510509138 A CN 201510509138A CN 105002467 B CN105002467 B CN 105002467B
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Abstract
The invention discloses a kind of Cu Ti amorphous alloy films and preparation method thereof, it is characterised in that：The structural formula of amorphous alloy film is CuxTi100‑x(54≤x≤66), wherein x are the atomic percentage of Cu elements；Unlike common preparation technology, the technology that the amorphous alloy film passes through electron beam+thermal resistance evaporation composite film coating, in preparation process, electron beam and thermal resistance evaporation source evaporation is respectively adopted in metal Ti and Ni metal, underlay substrate does not need heating/cooling device, preparation technology is simplified, reduces production cost.Noncrystal membrane prepared by the present invention, non crystalline structure is obvious, can control the composition and size of noncrystal membrane by adjusting evaporation electric current and evaporation time.
Description
Technical field
The invention belongs to amorphous alloy thin technology field of membrane materials, particularly relates to a kind of Cu-Ti amorphous alloy thins
Film and preparation method thereof.
Background technology
Non-crystaline amorphous metal is a kind of new metallic material for starting exploitation the last century 60's, with common crystal alloy phase
Than because it has more excellent mechanical property, magnetic performance, corrosion resistance and bio-compatibility, so as to receive material
The extensive concern in material field, and be considered to have and be extremely widely applied potentiality.
Amorphous alloy film not only has the excellent characteristics of block amorphous alloy, and because it is similar to two-dimensional material
Feature, prepares that required requirement is also lower, and glass forming ability scope is wider.In addition, amorphous alloy film have it is outstanding equal
Even property, wear-resisting and corrosion resistance, high rigidity, higher resistive, high activity and the property facilitated and many special magnetic properties.Because
Its excellent physical and chemical properties, the exploitation of nearest more than ten years amorphous alloy film, application development are rapid, especially it is micro-/receive
Electronic mechanical system (MEMS/NEMS) and biomedical sector, there is critically important potential using value.
Cu base noncrystal alloys are since being developed, because its relatively low cost and excellent mechanical property are by material
The concern in field, it is considered as specifically being widely applied prospect.At present, among the technique for preparing noncrystal membrane：1) magnetron sputtering
Method, its film prepared and substrate adhesion are more firm, but due to needing argon ion bombardment target using magnetron sputtering method, prepare sample
Product easily contain impurity, and need to prepare target, and operating process is complicated, and cost is higher；2) need to explore using the decrystallized reaction method of solid phase
Reaction time, reaction temperature, the Appropriate of monolayer film thickness, process is cumbersome, and preparation time is longer；3) twin-cathode ray beam is used
During evaporation, substrate can cause temperature higher because of the influence of two electron beam evaporation source heat radiations, typically using substrate cooling dress
Put.
The Cu-Ti amorphous alloy films prepared using electron beam+reactive evaporation, simple to operate, cost is cheap, has weight
The Research Significance wanted.
The content of the invention
The present invention is on the premise of the Forming ability and production cost of amorphous alloy film is considered, there is provided a kind of new
Cu-Ti amorphous alloy films and preparation method, it is amorphous to be obtained under the conditions of underlay substrate is without cooling device
Cu-Ti alloy firms.
The present invention solves technical problem, adopts the following technical scheme that
The Cu-Ti amorphous alloy films of the present invention, its feature are：The structural formula of the Cu-Ti amorphous alloy films is
CuxTi100-x(54≤x≤66), wherein x are the atomic percentage of Cu elements.
The specific preparation process of above-mentioned Cu-Ti amorphous alloy films is as follows：
(1) Cu blocks and Ti blocks are cut, Cu blocks and Ti blocks surface are polished, each 10min is cleaned successively with acetone and alcohol, blows
It is dry stand-by；
(2) using electron beam evaporation and thermal resistance evaporation composite film coating system, Ti blocks and Cu blocks are placed respectively as target
In electron beam evaporation copper crucible and thermal resistance evaporation tungsten boat, the substrate pallet that substrate is placed on above copper crucible
On, it is not necessary to cooling device；
(3) it is evacuated to 1 × 10-4Below Pa, regulation Electron Beam flow valuve is in 150~160mA, regulation resistance evaporation current
For 115~135A, make Ti and Cu while evaporate and be deposited on substrate, it is 1~4h to control sedimentation time, and producing deposition has Cu-
The substrate of Ti amorphous alloy films.
By adjusting Electron Beam flow valuve in the range of 150~160mA and thermal resistance evaporation being adjusted in the range of 115~135A
Electric current obtains the Cu-Ti amorphous alloy films of heterogeneity；Different-thickness is obtained by adjusting sedimentation time in the range of 1~4h
Cu-Ti amorphous alloy films.
The purity of raw material Ti blocks and Cu blocks is not less than 99.9wt.%.
Above-mentioned Cu-Ti amorphous alloy films are prepared using electron beam evaporation and thermal resistance evaporation composite film coating system, used
Unit type be：DZS-500 types electron beam/thermal resistance evaporation coating system, middle tech, Chinese (Shenyang).
The non crystalline structure characteristic of above-mentioned Cu-Ti amorphous alloy films is detected using X-ray diffraction method (XRD), device therefor
Model：X ' Pert Pro MPD X-ray diffractometers, PANalytical (Panalytical), Holland.
The surface topography and composition of above-mentioned Cu-Ti amorphous alloy films use field emission scanning electron microscope (FE-SEM)
And subsidiary energy disperse spectroscopy (EDS) detection, device therefor model：SU8020, FDAC, Japan.
Beneficial effects of the present invention are embodied in：
(1) Cu-Ti amorphous alloy films of the invention can prepare noncrystalline membrane in wider composition range, and
And the composition of noncrystal membrane and thickness can be controlled by adjusting Electron Beam flow valuve, thermal resistance evaporation electric current and evaporation time；
(2) Cu-Ti amorphous alloy films of the invention add the technology of thermal resistance evaporation composite film coating using electron beam, are preparing
During, electron beam evaporation source and thermal resistance evaporation source evaporation is respectively adopted in metal Ti and Ni metal, and underlay substrate need not add cold
But device, preparation technology is simplified, reduces production cost.
Brief description of the drawings
Fig. 1 is the XRD of alloy firm prepared by embodiment 1-5, and experiment uses the K of Cu targetsαRay；
Fig. 2 is the SEM surface topography maps of alloy firm prepared by embodiment 2；
Fig. 3 is the SEM end face shape figures of alloy firm prepared by embodiment 2.
Embodiment
Embodiment 1：Cu82Ti18The preparation of alloy firm
Step 1：By raw material Ti (99.9wt%), surface scale is removed in Cu (99.9wt%) polishings, and passes through acetone,
After alcohol is cleaned by ultrasonic each 10min, be respectively placed in copper crucible with tungsten boat, by substrate sheet glass with silicon chip through acetone, alcohol, go
After ionized water is cleaned by ultrasonic each 10min, drying is placed on substrate pallet；
Step 2：Put air valve into, open cooling water, blast pipe is placed in outside window, open filming equipment general supply, open mechanical pump electricity
Source, opening is other to take out valve, opens vacuum meter, when vacuum is less than 10Pa, closes side and takes out valve, opening magnetic valve, open slide valve,
Molecular pump power source is opened, when vacuum is less than 1 × 10-4During Pa, electron gun power supply is opened, presses scanning key, filament supply of shooting, is adjusted
For 0.3A, preheat 5 minutes, line control is adjusted to manually, opens high pressure 6KV, checks that whether line is minimum on manual instrument, is pressed
High pressure key, stablize 2 minutes, increase line to 25mA, regulation facula position clockwise and be located in crucible, be slowly increased line
To 150mA, thermal resistance evaporation power supply is opened, electric current is slowly increased to 135A, opens substrate rotary switch, it is revolved with 20r/min
Turn, open baffle plate, deposition is closed after 2 hours；
Step 3：Its composition is detected by energy disperse spectroscopy to sample obtained by above-mentioned steps 2, it is known that the composition of gained sample is put down
It is Cu82Ti18；
Step 4：Its structure is detected by XRD to sample obtained by above-mentioned steps 2, as shown in figure 1, there is obvious crystal
Peak, wherein first steamed bun peak is glass substrate Interference Peaks, second peak is the obvious sharpening of sample peak (40 °~50 °), explanation
The sample of preparation is partially-crystallized.
Embodiment 2：Cu66Ti34The preparation of amorphous alloy film
Step 1：By raw material Ti (99.9wt%), surface scale is removed in Cu (99.9wt%) polishings, and passes through acetone,
After alcohol is cleaned by ultrasonic each 10min, copper crucible is respectively placed in in tungsten boat, by substrate sheet glass and silicon chip through acetone, alcohol, going
After ionized water is cleaned by ultrasonic each 10min, drying is placed on substrate pallet；
Step 2：Put air valve into, open cooling water, blast pipe is placed in outside window, open filming equipment general supply, open mechanical pump electricity
Source, opening is other to take out valve, opens vacuum meter, when vacuum is less than 10Pa, closes side and takes out valve, opening magnetic valve, open slide valve,
Molecular pump power source is opened, when vacuum is less than 1 × 10-4During Pa, electron gun power supply is opened, presses scanning key, filament supply of shooting, is adjusted
For 0.3A, preheat 5 minutes, line control is adjusted to manually, opens high pressure 6KV, checks that whether line is minimum on manual instrument, is pressed
High pressure key, stablize 2 minutes, increase line to 25mA, regulation facula position clockwise and be located in crucible, be slowly increased line
To 155mA, thermal resistance evaporation power supply is opened, electric current is slowly increased to 130A, opens substrate rotary switch, it is revolved with 20r/min
Turn, open baffle plate, deposition is closed after 2 hours；
Step 3：Its composition is detected by energy disperse spectroscopy to sample obtained by above-mentioned steps 2, it is known that the composition of gained sample is put down
It is Cu66Ti34Non-crystaline amorphous metal；
Step 4：Its structure is detected by XRD to sample obtained by above-mentioned steps 2, as shown in figure 1, not occurring obvious
Crystal peak, wherein first steamed bun peak is glass substrate Interference Peaks, second steamed bun peak is sample peak (40 °~50 °), illustrates system
Standby sample amorphous structure.
Step 5：Its surface topography is detected by SEM to the sample prepared by above-mentioned steps 2, as shown in Fig. 2 film surface
Smooth densification, without obvious crackle.
Step 6：Its thickness is detected by SEM to the sample prepared by above-mentioned steps 2, as shown in figure 3, the film is about
236nm。
Embodiment 3：Cu60Ti40The preparation of amorphous alloy film
Step 1：By raw material Ti (99.9wt%), surface scale is removed in Cu (99.9wt%) polishings, and passes through acetone,
After alcohol is cleaned by ultrasonic each 10min, copper crucible is respectively placed in in tungsten boat, by substrate sheet glass and silicon chip through acetone, alcohol, going
After ionized water is cleaned by ultrasonic each 10min, drying is placed on substrate pallet；
Step 2：Put air valve into, open cooling water, blast pipe is placed in outside window, open filming equipment general supply, open mechanical pump electricity
Source, opening is other to take out valve, opens vacuum meter, when vacuum is less than 10Pa, closes side and takes out valve, opening magnetic valve, open slide valve,
Molecular pump power source is opened, when vacuum is less than 1 × 10-4During Pa, electron gun power supply is opened, presses scanning key, filament supply of shooting, is adjusted
For 0.3A, preheat 5 minutes, line control is adjusted to manually, opens high pressure 6KV, checks that whether line is minimum on manual instrument, is pressed
High pressure key, stablize 2 minutes, increase line to 25mA, regulation facula position clockwise and be located in crucible, be slowly increased line
To 155mA, thermal resistance evaporation power supply is opened, electric current is slowly increased to 125A, opens substrate rotary switch, it is revolved with 20r/min
Turn, open baffle plate, deposition is closed after 2 hours；
Step 3：Its composition is detected by energy disperse spectroscopy to sample obtained by above-mentioned steps 2, it is known that the composition of gained sample is put down
It is Cu60Ti40；
Step 4：Its structure is detected by XRD to sample obtained by above-mentioned steps 2, as shown in figure 1, not occurring obvious
Crystal peak, wherein first steamed bun peak is glass substrate Interference Peaks, second steamed bun peak is sample peak (40 °~50 °), illustrates system
Standby sample amorphous structure.
Embodiment 4：Cu59Ti41The preparation of amorphous alloy film
Step 1：By raw material Ti (99.9wt%), surface scale is removed in Cu (99.9wt%) polishings, and passes through acetone,
After alcohol is cleaned by ultrasonic each 10min, copper crucible is respectively placed in in tungsten boat, by substrate sheet glass and silicon chip through acetone, alcohol, going
After ionized water is cleaned by ultrasonic each 10min, drying is placed on substrate pallet；
Step 2：Put air valve into, open cooling water, blast pipe is placed in outside window, open filming equipment general supply, open mechanical pump electricity
Source, opening is other to take out valve, opens vacuum meter, when vacuum is less than 10Pa, closes side and takes out valve, opening magnetic valve, open slide valve,
Molecular pump power source is opened, when vacuum is less than 1 × 10-4During Pa, electron gun power supply is opened, presses scanning key, filament supply of shooting, is adjusted
For 0.3A, preheat 5 minutes, line control is adjusted to manually, opens high pressure 6KV, checks that whether line is minimum on manual instrument, is pressed
High pressure key, stablize 2 minutes, increase line to 25mA, regulation facula position clockwise and be located in crucible, be slowly increased line
To 160mA, thermal resistance evaporation power supply is opened, electric current is slowly increased to 125A, opens substrate rotary switch, it is revolved with 20r/min
Turn, open baffle plate, deposition is closed after 2 hours；
Step 3：Its composition is detected by energy disperse spectroscopy to sample obtained by above-mentioned steps 2, it is known that the composition of gained sample is put down
It is Cu59Ti41；
Step 4：Its structure is detected by XRD to sample obtained by above-mentioned steps 2, as shown in figure 1, not occurring obvious
Crystal peak, wherein first steamed bun peak is glass substrate Interference Peaks, second steamed bun peak is sample peak (30 °~45 °), illustrates system
Standby sample amorphous structure.
Embodiment 5：Cu54Ti46The preparation of amorphous alloy film
Step 1：By raw material Ti (99.9wt%), surface scale is removed in Cu (99.9wt%) polishings, and passes through acetone,
After alcohol is cleaned by ultrasonic each 10min, copper crucible is respectively placed in in tungsten boat, by substrate sheet glass and silicon chip through acetone, alcohol, going
After ionized water is cleaned by ultrasonic each 10min, drying is placed on substrate pallet；
Step 2：Put air valve into, open cooling water, blast pipe is placed in outside window, open filming equipment general supply, open mechanical pump electricity
Source, opening is other to take out valve, opens vacuum meter, when vacuum is less than 10Pa, closes side and takes out valve, opening magnetic valve, open slide valve,
Molecular pump power source is opened, when vacuum is less than 1 × 10-4During Pa, electron gun power supply is opened, presses scanning key, filament supply of shooting, is adjusted
For 0.3A, preheat 5 minutes, line control is adjusted to manually, opens high pressure 6KV, checks that whether line is minimum on manual instrument, is pressed
High pressure key, stablize 2 minutes, increase line to 25mA, regulation facula position clockwise and be located in crucible, be slowly increased line
To 160mA, thermal resistance evaporation power supply is opened, electric current is slowly increased to 120A, opens substrate rotary switch, it is revolved with 20r/min
Turn, open baffle plate, deposition is closed after 2 hours；
Step 3：Its composition is detected by energy disperse spectroscopy to sample obtained by above-mentioned steps 2, it is known that the composition of gained sample is put down
It is Cu54Ti46；
Step 4：Its structure is detected by XRD to sample obtained by above-mentioned steps 2, as shown in figure 1, not occurring obvious
Crystal peak, wherein first steamed bun peak is glass substrate Interference Peaks, second steamed bun peak is sample peak (40 °~50 °), illustrates system
Standby sample amorphous structure.
Claims (2)
1. a kind of preparation method of Cu-Ti amorphous alloy films, the structural formula of the Cu-Ti amorphous alloy films are
CuxTi100-x, 54≤x≤66, wherein x are the atomic percentage of Cu elements, it is characterised in that are comprised the following steps：
(1) Cu blocks and Ti blocks are cut, Cu blocks and Ti blocks surface are polished, clean each 10min successively with acetone and alcohol, drying is treated
With；
(2) using electron beam evaporation and thermal resistance evaporation composite film coating system, Ti blocks and Cu blocks are individually positioned in electricity as target
In beamlet evaporation copper crucible and thermal resistance evaporation tungsten boat, substrate is placed on the substrate pallet above copper crucible；
(3) it is evacuated to 1 × 10-4Below Pa, regulation Electron Beam flow valuve are in 150~160mA, regulation resistance evaporation current
115~135A, make Ti and Cu while evaporate and be deposited on substrate, it is 1~4h to control sedimentation time, and producing deposition has Cu-Ti
The substrate of amorphous alloy film；
By adjusting Electron Beam flow valuve in the range of 150~160mA and thermal resistance evaporation electric current being adjusted in the range of 115~135A
Obtain the Cu-Ti amorphous alloy films of heterogeneity；Different-thickness is obtained by adjusting sedimentation time in the range of 1~4h
Cu-Ti amorphous alloy films.
2. preparation method according to claim 1, it is characterised in that：The purity of raw material Ti blocks and Cu blocks is not less than
99.9wt.%.
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