CN107881475A - A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method - Google Patents
A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method Download PDFInfo
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- CN107881475A CN107881475A CN201610871554.8A CN201610871554A CN107881475A CN 107881475 A CN107881475 A CN 107881475A CN 201610871554 A CN201610871554 A CN 201610871554A CN 107881475 A CN107881475 A CN 107881475A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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Abstract
The invention provides a kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method, its step is：(1) target is chosen：Stoichiometrically choose NiMnTi alloys targets and Co simple substance targets；(2) cosputtering：1. substrate heats：The alloys target chosen and simple substance target are placed on the sputtering target of sputtering chamber and fixed, chamber lid is closed and is evacuated down to 10‑4Heating substrate after below Pa, opens substrate heating power supply, and adjustment heating knob is begun to warm up to correct position；2. sputter chamber pressure adjustment：The argon gas that purity is 99.999% is filled with, suitable size is arrived by force by adjusting flow instrument and slide valve control sputtering intraventricular pressure；3. DC sputturing method：The power knob for adjusting sputtering target starts cosputtering to OK range, stops sputtering after sputtering certain time.
Description
Technical field
The present invention relates to Ni-Co-Mn-Ti alloy firms, especially provide one kind and are prepared by magnetron sputtering DC sputturing method
The method of Ni-Co-Mn-Ti alloy firms.
Background technology
Ni-Mn-X (X=In, Sn, Sb, Ga, Al) ferromagnetic shape memory alloys (FSMAs) are one to receive much concern in recent years
Class novel intelligent material, while there is thermoelasticity and ferromagnetic shape memory effect, therefore, such alloy has big recovery concurrently should
Become, export stress, high response frequency greatly and the overall characteristic such as accurately control, allow it in high-power underwater sonar, microbit
Moving the field such as device, vibrations and Noise measarement, linear motor, microwave device, robot has important application.In addition, such alloy is also
With big magnetothermal effect, piezocaloric effect, play fuel factor, magneto-resistance effect, magneto-strain, exchange biased, giant Hall effect etc.
Multi-functional property, also all there is potential application background in many fields such as refrigeration, magnetic recording.Except block and Tape samples
Outside, with the development of technology, to device miniaturization and large buffer memory it is required that film sample has bigger development prospect
And the market demand.
Sputtering technology is one kind of physical vapour deposition (PVD), is a kind of important method for preparing thin-film material.Magnetron sputtering skill
Art is exactly to be so as to control the motion of electronics in electric field with reference to magnetic control principle and sputtering technology and using the stationary distribution in magnetic field
Optimization to sputtering technology.With the in-depth that MEMS (MEMS) is studied and applied, the local refrigeration in short space will
Important application is obtained in MEMS system.In order to adapt to the space layout of the development trend of miniaturization and microminiaturization, under low field
The thin-film material become with high magnetic entropy will be widely used.But current research work focuses primarily upon bulk and bar
Band, the research of thin-film material are also relatively fewer.To find out its cause, the preparation of magnetic membrane material is a very big difficulty, at present
The preparation of magnetic membrane material, due to preparing magnetic membrane material using magnetron sputtering method, is made frequently with the method for magnetron sputtering
For the film gone out, not only quality is good, used device is moderate, and output efficiency is high, and can obtain height under low operating pressure
Deposition, high-quality thin film can also be obtained under low base reservoir temperature.But the composition of alloy firm is often not true before sputtering
Fixed, and different alloy firm composition and film thickness will be obtained using different parameter settings in sputtering.
Traditional Ni-Mn bases FSMAs is made up of transition element and main group member.In recent years, Ni-Co-Mn-Ti is this
The Ni-Mn bases FSMAs being all made up of transition element is found.Although traditional Ni-Mn base FSMAs film samples have been ground
Study carefully, but Ni-Co-Mn-Ti alloy firms also nobody's report and research.Know according to the research of existing block, Ni-Co-Mn-Ti
As a kind of new Ni-Mn bases FSMAs, there is big magnetothermal effect, magneto-resistor and big recoverable strain and quick response
Performance, so having very big application prospect in refrigeration and smart field.Its thin-film material is even more to be expected in micro- refrigeration, micro sensing
It is used widely in the high-tech areas such as device, microdrive, therefore is highly desirable to carry out Ni-Co-Mn-Ti alloy firms
Prepare and in-depth study is carried out to its performance.The present invention is based on this purpose and proposes that one kind is splashed altogether by magnetron sputtering direct current
Shooting method prepares Ni-Co-Mn-Ti alloy firms.
The content of the invention
Ni-Co-Mn-Ti alloy firms are prepared by magnetron sputtering DC sputturing method it is an object of the invention to provide one kind
Method, this method has simple and convenient, safe and efficient and low power consumption and other advantages.
The technical scheme is that：
A kind of method that Ni-Co-Mn-Ti alloy firms are prepared by magnetron sputtering cosputtering, it is characterised in that the side
Method comprises the following steps：
(1) target is chosen：Stoichiometrically choose NiMnTi alloy target materials and Co simple substance target carries out cosputtering, target
The diameter of material is all 60mm, and wherein the thickness of alloy target material is 3mm, and the thickness of Co simple substance targets is 1~2mm；
(2) substrate heats：The alloy target material chosen and Co simple substance targets are placed on the sputtering target of sputtering chamber fixed
It is good, close chamber lid and be evacuated down to 10-4Heating substrate after below Pa, open substrate heating power supply, adjustment heating knob to suitable position
Put and begin to warm up, heating temperature range is 200 DEG C~700 DEG C；
(3) chamber pressure adjustment is sputtered：Argon gas (argon gas that preferably purity is 99.999%) is filled with, by adjusting flow instrument
It is 0.25Pa~2.5Pa to control the sputtering strong scope of intraventricular pressure with slide valve；
(4) DC sputturing method：The power knob of adjustment sputtering target starts cosputtering, the sputtering of alloys target to OK range
Power is 30W~70W, and simple substance target sputtering power is 5W~30W, sputtering time 0.5h~2.5h.
Alloy target material described in step (1) and simple substance target purity are more than 99.95%；According to different stoichiometries
Than have chosen multiple targets, wherein the composition range of each element is respectively in alloys target：Ni (25~45), Mn (25~45), Ti
(5~25).
Substrate heating is that alloys target and simple substance target are individually placed to above two direct current targets of sputtering chamber described in step (2)
Fix, close chamber lid and start to vacuumize, be evacuated to pressure less than 10-4Substrate heating can be just carried out after Pa, design temperature is institute
Temperature is selected, adjustment heated current knob to 3~4A preheats 4~6 minutes, high current to 5~8A, and specific electric current regards selected temperature
Adjustment, makes temperature rapidly rise to assigned temperature.
It is first somewhat to fasten slide valve that chamber pressure adjustment is sputtered described in step (3), but is not related on earth, opens argon bottle
Master switch, adjustment pressure registration arrive 0.375MPa or so, open argon inlet valve, regulation flow instrument is 24 or so, is then passed through
Rotating sluice valve regulation sputtering intraventricular pressure is by force to required pressure.
DC sputturing method described in step (4) is the power that sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized
Knob, making alloys target and simple substance target, build-up of luminance carries out cosputtering simultaneously, now only opens target baffle plate without opening substrate baffle plate, in advance
10~15min is sputtered, substrate baffle plate is then opened and starts deposition film.
The beneficial effects of the invention are as follows：
The method of the invention is simple and convenient, it is not necessary to and the annealing heat-treats time, energy resource consumption is few, and environmental pollution is small,
It is low to prepare cost, is adapted to industrialized production.The Ni-Co-Mn-Ti alloy firm excellent performances obtained using this method, can conduct
Magneto-caloric material, the magnetic functional materials such as magneto-resistor can be even used as by exploring.
Brief description of the drawings
Ni-Co-Mn-Ti alloy firms surface SEM figures when Fig. 1 substrates heating-up temperature is 250 DEG C.
Ni-Co-Mn-Ti alloy firm XRDs when Fig. 2 substrates heating-up temperature is 250 DEG C.
Ni-Co-Mn-Ti alloy firms section SEM figures when Fig. 3 substrates heating-up temperature is 250 DEG C.
Ni-Co-Mn-Ti alloy firms surface SEM figures when Fig. 4 substrates heating-up temperature is 350 DEG C.
Ni-Co-Mn-Ti alloy firm XRDs when Fig. 5 substrates heating-up temperature is 350 DEG C.
Embodiment
Embodiment 1
(1) target is chosen：Stoichiometrically choose the Ni that purity is more than 99.95%25Mn30Ti21Alloys target and Co
Simple substance target carries out cosputtering, and the diameter of target is all 60mm, and wherein the thickness of alloys target is 3mm, and the thickness of Co targets is 1mm, no
Can be too thick；
(2) substrate heats：Alloys target and simple substance target are individually placed to fix above two direct current targets of sputtering chamber, closed
Closed chamber lid starts to be evacuated to pressure less than 10-4Substrate heating can be just carried out after Pa, design temperature is 250 DEG C, adjustment heating
Current knob preheats 6 minutes to 3A, high current to 6A, temperature is rapidly risen to 250 DEG C；
(3) chamber pressure adjustment is sputtered：Slide valve is somewhat first fastened, but is not related on earth, argon bottle master switch is opened, adjusts
Seamless power registration is filled with argon gas to 0.375MPa or so, purity of argon 99.999%, opens argon inlet valve, adjusts flow instrument
Value be 24 or so, then by rotating sluice valve regulation sputter intraventricular pressure arrive 0.30Pa by force；
(4) DC sputturing method：The power knob of sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized, makes conjunction
Build-up of luminance carries out cosputtering simultaneously for gold target and simple substance target, and the power of alloys target is 30W~70W, and the power of simple substance target is 5W~30W,
Target baffle plate is now only opened without opening substrate baffle plate, pre-sputtering 10min, substrate baffle plate is then opened and starts deposition film,
Deposit 1h.
Long-time high annealing is needed just to obtain single-phase alloy sample relative to cast alloy, this method avoids annealing
Heat treatment process, preparation cost is reduced, has saved the energy, overcome the shortcomings that block Tape samples are frangible, be adapted to industrialization
Production, it can freeze as magnetic is prepared, a kind of effective method of magneto-resistor equimagnetic functional material.The preparation of film is advantageous to
The miniaturization of device, represent the direction of future development.
Embodiment 2
(1) target is chosen：Stoichiometrically choose the Ni that purity is more than 99.95%45Mn36Ti10Alloys target and Co
Simple substance target carries out cosputtering, and the diameter of target is all 60mm, and wherein the thickness of alloys target is 3mm, and the thickness of Co targets is 1.5mm；
(2) substrate heats：Alloys target and simple substance target are individually placed to fix above two direct current targets of sputtering chamber, closed
Closed chamber lid starts to be evacuated to pressure less than 10-4Substrate heating can be just carried out after Pa, design temperature is 350 DEG C, adjustment heating
Current knob preheats 6 minutes to 3A, high current to 5A, temperature is rapidly risen to 350 DEG C；
(3) chamber pressure adjustment is sputtered：Slide valve is somewhat first fastened, but is not related on earth, argon bottle master switch is opened, adjusts
Seamless power registration is filled with argon gas to 0.375MPa or so, purity of argon 99.999%, opens argon inlet valve, adjusts flow instrument
Value be 24 or so, then by rotating sluice valve regulation sputter intraventricular pressure arrive 0.25Pa by force；
(4) DC sputturing method：The power knob of sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized, makes conjunction
Build-up of luminance carries out cosputtering simultaneously for gold target and simple substance target, and the power of alloys target is 30W~70W, and the power of simple substance target is 5W~30W,
Target baffle plate is now only opened without opening substrate baffle plate, pre-sputtering 15min, substrate baffle plate is then opened and starts deposition film,
Deposit 1.5h.
Embodiment 3
(1) target is chosen：Stoichiometrically choose the Ni that purity is more than 99.95%30Mn25Ti8Alloys target and Co are mono-
Matter target carries out cosputtering, and the diameter of target is all 60mm, and wherein the thickness of alloys target is 3mm, and the thickness of Co targets is 1.5mm；
(2) substrate heats：Alloys target and simple substance target are individually placed to fix above two direct current targets of sputtering chamber, closed
Closed chamber lid starts to be evacuated to pressure less than 10-4Substrate heating can be just carried out after Pa, design temperature is 450 DEG C, adjustment heating
Current knob preheats 5 minutes to 4A, high current to 8A, temperature is rapidly risen to 450 DEG C；
(3) chamber pressure adjustment is sputtered：Slide valve is somewhat first fastened, but is not related on earth, argon bottle master switch is opened, adjusts
Seamless power registration is filled with argon gas to 0.375MPa or so, purity of argon 99.999%, opens argon inlet valve, adjusts flow instrument
Value be 24 or so, then by rotating sluice valve regulation sputter intraventricular pressure arrive 2.0Pa by force；
(4) DC sputturing method：The power knob of sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized, makes conjunction
Build-up of luminance carries out cosputtering simultaneously for gold target and simple substance target, and the power of alloys target is 30W~70W, and the power of simple substance target is 5W~30W,
Target baffle plate is now only opened without opening substrate baffle plate, pre-sputtering 10min, substrate baffle plate is then opened and starts deposition film,
Deposit 2.5h.
Embodiment 4
(1) target is chosen：Stoichiometrically choose the Ni that purity is more than 99.95%35Mn45Ti24Alloys target and Co
Simple substance target carries out cosputtering, and the diameter of target is all 60mm, and wherein the thickness of alloys target is 3mm, and the thickness of Co targets is 2mm；
(2) substrate heats：Alloys target and simple substance target are individually placed to fix above two direct current targets of sputtering chamber, closed
Closed chamber lid starts to be evacuated to pressure less than 10-4Substrate heating can be just carried out after Pa, design temperature is 600 DEG C, adjustment heating
Current knob preheats 6 minutes to 3A, high current to 6A, temperature is rapidly risen to 600 DEG C；
(3) chamber pressure adjustment is sputtered：Slide valve is somewhat first fastened, but is not related on earth, argon bottle master switch is opened, adjusts
Seamless power registration is filled with argon gas to 0.375MPa or so, purity of argon 99.999%, opens argon inlet valve, adjusts flow instrument
Value be 24 or so, then by rotating sluice valve regulation sputter intraventricular pressure arrive 0.25Pa by force；
(4) DC sputturing method：The power knob of sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized, makes conjunction
Build-up of luminance carries out cosputtering simultaneously for gold target and simple substance target, and the power of alloys target is 30W~70W, and the power of simple substance target is 5W~30W,
Target baffle plate is now only opened without opening substrate baffle plate, pre-sputtering 10min, substrate baffle plate is then opened and starts deposition film,
Deposit 1.5h.
Embodiment 5
(1) target is chosen：Stoichiometrically choose the Ni that purity is more than 99.95%30Mn41Ti5Alloys target and Co are mono-
Matter target carries out cosputtering, and the diameter of target is all 60mm, and wherein the thickness of alloys target is 3mm, and the thickness of Co targets is 1mm, it is impossible to
It is too thick；
(2) substrate heats：Alloys target and simple substance target are individually placed to fix above two direct current targets of sputtering chamber, closed
Closed chamber lid starts to be evacuated to pressure less than 10-4Substrate heating can be just carried out after Pa, design temperature is 700 DEG C, adjustment heating
Current knob preheats 6 minutes to 3A, high current to 8A, temperature is rapidly risen to 700 DEG C；
(3) chamber pressure adjustment is sputtered：Slide valve is somewhat first fastened, but is not related on earth, argon bottle master switch is opened, adjusts
Seamless power registration is filled with argon gas to 0.375MPa or so, purity of argon 99.999%, opens argon inlet valve, adjusts flow instrument
Value be 24 or so, then by rotating sluice valve regulation sputter intraventricular pressure arrive 0.50Pa by force；
(4) DC sputturing method：The power knob of sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized, makes conjunction
Build-up of luminance carries out cosputtering simultaneously for gold target and simple substance target, and the power of alloys target is 30W~70W, and the power of simple substance target is 5W~30W,
Target baffle plate is now only opened without opening substrate baffle plate, pre-sputtering 10min, substrate baffle plate is then opened and starts deposition film,
Deposit 0.5h.
Although introducing and describing the embodiment of the present invention, the invention is not limited in this, but can also
Implemented with the other modes in the range of the technical scheme defined in appended claims, such as can also by adjusting target
The sputtering power of material controls the composition of film and thickness, by adjust temperature change film into phase situation, regulation sputtering
Time changes film thickness etc..Any equivalent change or modification in accordance with the spirit of the invention, it should all cover in this hair
Within bright protection domain.
Claims (5)
- A kind of 1. method that Ni-Co-Mn-Ti alloy firms are prepared by magnetron sputtering cosputtering, it is characterised in that methods described Comprise the following steps：(1) target is chosen：Stoichiometrically choose NiMnTi alloy target materials and Co simple substance target carries out cosputtering, target Diameter is all 60mm, and wherein the thickness of alloy target material is 3mm, and the thickness of Co simple substance targets is 1~2mm；(2) substrate heats：The alloy target material chosen and Co simple substance targets are placed on the sputtering target of sputtering chamber and fixed, is closed Closed chamber lid is evacuated down to 10-4Below Pa, heats substrate, and heating-up temperature is 200 DEG C~700 DEG C；(3) chamber pressure adjustment is sputtered：Argon gas is filled with, by adjusting flow instrument and slide valve controls the sputtering strong scope of intraventricular pressure to be 0.25Pa~2.5Pa；(4) DC sputturing method：The sputtering power of alloys target is 30W~70W, and simple substance target sputtering power is 5W~30W, during sputtering Between 0.5h~2.5h.
- 2. according to the method for preparing Ni-Co-Mn-Ti alloy firms described in claim 1 by magnetron sputtering cosputtering, its feature It is：Described target purity is more than 99.95%, and wherein the atomic ratio of each composition is in NiMnTi alloy target materials：Ni 25~ 45, Mn 25~45, Ti 5~25.
- 3. according to the method for preparing Ni-Co-Mn-Ti alloy firms described in claim 1 by magnetron sputtering cosputtering, its feature It is：Step (2) first adjusts heated current knob to 3~4A preheatings 4~6 minutes, high current to 5 before carrying out substrate heating ~8A, specific electric current regard selected temperature and adjusted, and temperature is rapidly risen to assigned temperature.
- 4. according to the method for preparing Ni-Co-Mn-Ti alloy firms described in claim 1 by magnetron sputtering cosputtering, its feature It is：It is first somewhat to fasten slide valve that chamber pressure adjustment is sputtered described in step (3), but is not related on earth, opens argon bottle and always opens Close, adjustment pressure registration to 0.375MPa, open argon inlet valve, regulation flow instrument is 24, is then adjusted by rotating gate plate valve Section sputtering intraventricular pressure is by force to required pressure.
- 5. according to the method for preparing Ni-Co-Mn-Ti alloy firms described in claim 1 by magnetron sputtering cosputtering, its feature It is：DC sputturing method described in step (4) is the power rotation that sputtering target is adjusted after sputtering intraventricular pressure is strong and temperature is all stablized Button, making alloys target and simple substance target, build-up of luminance carries out cosputtering simultaneously, now only opens target baffle plate without opening substrate baffle plate, splashes in advance 10~15min is penetrated, substrate baffle plate is then opened and starts deposition film.
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Cited By (5)
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| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient heat-sensitive film |
| CN109913816A (en) * | 2019-04-29 | 2019-06-21 | 天津城建大学 | Temperature gradient magneto-caloric material and preparation method thereof |
| CN112663002A (en) * | 2020-09-04 | 2021-04-16 | 中科传感(佛山)科技有限公司 | Thermistor film preparation method based on direct-current reactive co-sputtering |
| CN113235055A (en) * | 2021-05-07 | 2021-08-10 | 杭州电子科技大学 | Ni-Mn-Ti-based multi-element alloy target material and preparation method and film thereof |
| CN114959613A (en) * | 2022-06-15 | 2022-08-30 | 西安热工研究院有限公司 | Method for enhancing corrosion resistance of medium-entropy alloy CoCrNi film |
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| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient heat-sensitive film |
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| CN114959613A (en) * | 2022-06-15 | 2022-08-30 | 西安热工研究院有限公司 | Method for enhancing corrosion resistance of medium-entropy alloy CoCrNi film |
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