CN109437318A - A kind of preparation method of extension hexad ferrite nano-dot matrix structure - Google Patents
A kind of preparation method of extension hexad ferrite nano-dot matrix structure Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of extension hexad ferrite nano-dot matrix structure, the Ferrite Material in the present invention has molecular formula: AFe12‑xMxO19, wherein A is at least one of Ba element or Sr element, and M is Sc element, and x is the atomic ratio content of M: 1.78 < x≤1.9.With high-purity BaCO3、SrCO3、Fe2O3,Sc2O3Powder is raw material, by the atomic molar in molecular formula than proportion, it is put into after mixing raw material after weighing in ball mill and carries out ball milling, target is obtained after drying grinding, then nanoporous template resistant to high temperature is used, foraminous die plate absorption is covered in monocrystal chip surface, nanostructure preparation uses pulse laser deposition plating technology, substrate temperature when nano structure membrane is grown is 650-850 DEG C, rate of temperature fall after nano structure membrane has been grown is 15-40 DEG C/min, cooling air pressure is oxygen, and oxygen pressure is 15kPa-0.8MPa；Nanoporous template resistant to high temperature is removed, hexad ferrite nano-structure array is obtained.
Description
Technical field
The present invention relates to a kind of preparation methods of extension hexad ferrite nano-dot matrix structure, belong to Ferrite Material technology
Field.
Background technique
Hexad ferrite has preferable chemical stability and corrosion resistance, while also having high-coercive force and Curie temperature
The advantages that, it can be used as permanent-magnet material, while can also store in information, microwave information transmission (circulator), radar detection, suction
The fields such as wave are with a wide range of applications.The preparation method of hexad ferrite film has been widely studied and has reported at present.
Ferrite nano structure is mainly prepared by chemical solution method.Certain ferritic proportioning components chemical solution is pressed, then high temperature
Heating generates chemical reaction in the solution, then prepares ferrite nano structure by control reaction time and temperature.With device
The development of part miniaturization needs to use the iron oxygen with crystal structure and magnetic height preferred orientation in certain miniature magnetoelectronic devices
Body nanostructure.Crystal structure and magnetic height in the single-phase ferrite nano structure for the chemical solution method preparation reported at present
Preferred orientation is all weaker, substantially the ferrite nano structure without preferred orientation.
Summary of the invention
The purpose of the present invention is to solve above-mentioned described problems in the prior art, provide a kind of extension hexad ferrite
The preparation method of nano-dot matrix structure.
The present invention adopts the following technical scheme: a kind of preparation method of extension hexad ferrite nano-dot matrix structure, including
Following steps:
(1) Ferrite Material in the present invention has molecular formula: AFe12-xMxO19, wherein A is in Ba element or Sr element
At least one, M be Sc element, the numberical range of x are as follows: 1.78 x≤1.9 <.With high-purity BaCO3、SrCO3、Fe2O3,Sc2O3Powder
End is that raw material is put into ball mill after mixing raw material after weighing by the atomic molar in molecular formula than proportion and carries out ball milling；
(2) it is put into dryer and dries after the completion of ball milling, dryer temperature is 70-100 DEG C, and drying time is 30-50 points
Clock；
(3) raw material grind after drying is placed in crucible, is put into tube furnace and carries out preheating；Tube furnace is according to temperature
Gradient increased temperature is spent, heating rate is 2 DEG C/min, and calcined temperature is 800-1000 DEG C, and burn-in time is 17-24 hours, is pre-sintered
Rate of temperature fall after beam is 1-3 DEG C/min；
(4) 3-5 drop PET is instilled hand lapping 20-40 minutes after the completion of pre-burning, in pre-burning medicine powder bonds glue, then
Secondary grinding is not obviously bonded up to no caking phenomenon and with mortar wall；
(5) powder is poured into mold, pressurization 5-10MPa keeps 10-15min, and molded samples are taken out after decompression, observes
Sample is with the presence or absence of slight crack etc., and slight crack is then needed to grind again as powder and suppressed until flawless again if it exists；
(6) molded samples are put into sintering processes in tube furnace, tube furnace heats up according to temperature gradient, heating rate 2
DEG C/min, sintering temperature is 1220 DEG C, and sintering time is 17-24 hours, and the rate of temperature fall after the completion of being sintered is 1-3 DEG C/min；
(7) molded samples are taken out after the completion of being sintered, target rim and surface are carefully ground using sand paper, by table
Face polishes smooth to obtain the target of preparation extension nanostructure；
(8) nanoporous template resistant to high temperature is used, foraminous die plate absorption is covered in monocrystal chip surface, nanostructure
Preparation uses pulse laser deposition plating technology, and background vacuum pressure is higher than 2 × 10-4Pa；
(9) substrate temperature when nano structure membrane is grown is 650-850 DEG C, and the speed of rotation of substrate is 1-3R/min,
The distance between substrate and target are 7-10cm, and the target speed of rotation is 6-10R/min, and the power of pulse laser is 10-
100mJ/cm2, frequency 2-10Hz, the rate of temperature fall after nano structure membrane has been grown is 15-40 DEG C/min, and cooling air pressure is
Oxygen, oxygen pressure are 15kPa-0.8MPa；Nanoporous template resistant to high temperature is removed, hexad ferrite nanostructure battle array is obtained
Column；
(10) the after annealing temperature of nano-structure array are as follows: 1050-1250 DEG C, heating rate is 2-5 DEG C/min, cooling speed
Rate is 1-3 DEG C/min.
Further, drum's speed of rotation is 200-300R/min in the step (1), and Ball-milling Time is 10-20 hours.
It further, is air or flowing oxygen atmosphere in the tube furnace in the step (3).
Further, the monocrystal chip is single crystalline Si substrate, Si/Pt substrate, monocrystalline Al2O3Substrate or monocrystalline SrTiO3
One of substrate.
Further, atmosphere when nano structure membrane is grown in the step (9) is flowing oxygen, and oxygen pressure is 5-
25Pa, flow rate 15-40sccm.
Further, after annealing atmosphere is flowing oxygen in the step (10), and oxygen pressure is 5-30Pa, and flow rate is
15-40sccm。
Preparation method of the present invention is simple, and step is easily operated, and preparation cost is lower, the extension hexad ferrite being prepared
Nano-dot matrix structure, size and density are able to carry out accurate control；There is epitaxial relationship between ferrite nano structure and substrate,
To guarantee magnetic anisotropy outside good face
Detailed description of the invention
Fig. 1 is the XRD diagram of extension hexad ferrite nano-dot matrix structure in the embodiment of the present invention two.
Fig. 2 is the scanning electron microscope schematic diagram in the embodiment of the present invention two.
Fig. 3 is the magnetism testing result figure in the embodiment of the present invention two.
Specific embodiment
Below in conjunction with attached drawing, the invention will be further described.
Embodiment 1:
A kind of preparation method of extension hexad ferrite nano-dot matrix structure, includes the following steps:
(1) Ferrite Material in the present invention has molecular formula: SrFe10.22Sc1.78O19, with high-purity BaCO3、SrCO3、
Fe2O3,Sc2O3Powder is raw material, by the atomic molar in molecular formula than proportion, is put into ball mill after mixing raw material after weighing
Middle carry out ball milling, drum's speed of rotation 200R/min, Ball-milling Time are 15 hours；
(2) it is put into dryer and dries after the completion of ball milling, dryer temperature is 70 DEG C, drying time 50 minutes；
(3) raw material grind after drying is placed in crucible, is put into tube furnace and carries out preheating；Tube furnace is according to temperature
Gradient increased temperature is spent, heating rate is 2 DEG C/min, and calcined temperature is 800 DEG C, and burn-in time is 17 hours, the drop after pre-burning
Warm rate is 1 DEG C/min, is air or flowing oxygen atmosphere in tube furnace；
(4) hand lapping 40 minutes after the completion of pre-burning instill 3 drop PET in pre-burning medicine powder and bond glue, regrinding
It is not obviously bonded up to no caking phenomenon and with mortar wall；
(5) powder is poured into mold, pressurization 5MPa keeps 15min, and molded samples are taken out after decompression, and observation sample is
It is no there are slight crack etc., if it exists slight crack then need to grind again as powder and again compacting until flawless；
(6) molded samples are put into sintering processes in tube furnace, tube furnace heats up according to temperature gradient, heating rate 2
DEG C/min, sintering temperature is 1220 DEG C, and sintering time is 17 hours, and the rate of temperature fall after the completion of being sintered is 1 DEG C/min；
(7) molded samples are taken out after the completion of being sintered, target rim and surface are carefully ground using sand paper, by table
Face polishes smooth to obtain the target of preparation extension nanostructure；
(8) nanoporous template resistant to high temperature is used, foraminous die plate absorption is covered in monocrystal chip surface, monocrystal chip
For single crystalline Si substrate, Si/Pt substrate, monocrystalline Al2O3One of substrate or monocrystalline SrTiO3 substrate, nanostructure preparation use
Pulse laser deposition plating technology, background vacuum pressure are higher than 2 × 10-4Pa；
(9) substrate temperature when nano structure membrane is grown is 650 DEG C, and the speed of rotation of substrate is 3R/min, substrate with
The distance between target is 7cm, and the target speed of rotation is 10R/min, and the power of pulse laser is 10mJ/cm2, frequency is
10Hz, the rate of temperature fall after nano structure membrane has been grown is 15 DEG C/min, and cooling air pressure is oxygen, and oxygen pressure is 15kPa；It goes
Except nanoporous template resistant to high temperature, hexad ferrite nano-structure array is obtained, atmosphere when nano structure membrane is grown is
Oxygen is flowed, oxygen pressure is 25Pa, flow rate 15sccm；
(10) the after annealing temperature of nano-structure array are as follows: 1050 DEG C, heating rate is 5 DEG C/min, rate of temperature fall 1
DEG C/min, after annealing atmosphere is flowing oxygen, and oxygen pressure is 30Pa, flow rate 15sccm.
Embodiment 2:
A kind of preparation method of extension hexad ferrite nano-dot matrix structure, includes the following steps:
(1) Ferrite Material in the present invention has molecular formula: BaFe10.2Sc1.8O19, with high-purity BaCO3、SrCO3、
Fe2O3,Sc2O3Powder is raw material, by the atomic molar in molecular formula than proportion, is put into ball mill after mixing raw material after weighing
Middle carry out ball milling, drum's speed of rotation 200R/min, Ball-milling Time are 15 hours；
(2) it is put into dryer and dries after the completion of ball milling, dryer temperature is 90 DEG C, and drying time is 40 minutes；
(3) raw material grind after drying is placed in crucible, is put into tube furnace and carries out preheating；Tube furnace is according to temperature
Gradient increased temperature is spent, heating rate is 2 DEG C/min, and calcined temperature is 900 DEG C, and burn-in time is 15 hours, the drop after pre-burning
Warm rate is 2 DEG C/min, is air or flowing oxygen atmosphere in tube furnace；
(4) hand lapping 30 minutes after the completion of pre-burning instill 4 drop PET in pre-burning medicine powder and bond glue, regrinding
It is not obviously bonded up to no caking phenomenon and with mortar wall；
(5) powder is poured into mold, pressurization 8MPa keeps 12min, and molded samples are taken out after decompression, and observation sample is
It is no there are slight crack etc., if it exists slight crack then need to grind again as powder and again compacting until flawless；
(6) molded samples are put into sintering processes in tube furnace, tube furnace heats up according to temperature gradient, heating rate 2
DEG C/min, sintering temperature is 1220 DEG C, and sintering time is 17 hours, and the rate of temperature fall after the completion of being sintered is 2 DEG C/min；
(7) molded samples are taken out after the completion of being sintered, target rim and surface are carefully ground using sand paper, by table
Face polishes smooth to obtain the target of preparation extension nanostructure；
(8) nanoporous template resistant to high temperature is used, foraminous die plate absorption is covered in monocrystal chip surface, monocrystal chip
For single crystalline Si substrate, Si/Pt substrate, monocrystalline Al2O3Substrate or monocrystalline SrTiO3One of substrate, nanostructure preparation use
Pulse laser deposition plating technology, background vacuum pressure are higher than 2 × 10-4Pa；
(9) substrate temperature when nano structure membrane is grown is 850 DEG C, the speed of rotation 2R/min of substrate, substrate and target
The distance between material is 8cm, and the target speed of rotation is 8R/min, and the power of pulse laser is 80mJ/cm2, frequency 5Hz receives
Rate of temperature fall after rice structural membrane has been grown is 30 DEG C/min, and cooling air pressure is oxygen, and oxygen pressure is 0.5MPa；Remove resistance to height
The nanoporous template of temperature obtains hexad ferrite nano-structure array, and atmosphere when nano structure membrane is grown is flowing oxygen
Gas, oxygen pressure are 20Pa, flow rate 30sccm；
(10) the after annealing temperature of nano-structure array are as follows: 1200 DEG C, heating rate is 3 DEG C/min, rate of temperature fall 2
DEG C/min, after annealing atmosphere is flowing oxygen, and oxygen pressure is 20Pa, flow rate 30sccm.
Embodiment 3:
A kind of preparation method of extension hexad ferrite nano-dot matrix structure, includes the following steps:
(1) Ferrite Material in the present invention has molecular formula: BaSrFe10.1Sc1.9O19, rub by the atom in molecular formula
You are put into ball mill after mixing raw material after weighing than proportion and carry out ball milling, drum's speed of rotation 200R/min, Ball-milling Time
It is 15 hours；
(2) it is put into dryer and dries after the completion of ball milling, dryer temperature is 100 DEG C, and drying time is 30 minutes；
(3) raw material grind after drying is placed in crucible, is put into tube furnace and carries out preheating；Tube furnace is according to temperature
Gradient increased temperature is spent, heating rate is 2 DEG C/min, and calcined temperature is 1000 DEG C, and burn-in time is 17 hours, the drop after pre-burning
Warm rate is 3 DEG C/min, is air or flowing oxygen atmosphere in tube furnace；
(4) hand lapping 20 minutes after the completion of pre-burning instill 5 drop PET in pre-burning medicine powder and bond glue, regrinding
It is not obviously bonded up to no caking phenomenon and with mortar wall；
(5) powder is poured into mold, pressurization 10MPa keeps 10min, and molded samples are taken out after decompression, observes sample
With the presence or absence of slight crack etc., if it exists slight crack then need to grind again as powder and again compacting until flawless；
(6) molded samples are put into sintering processes in tube furnace, tube furnace heats up according to temperature gradient, heating rate 2
DEG C/min, sintering temperature is 1050 DEG C, and sintering time is 17 hours, and the rate of temperature fall after the completion of being sintered is 3 DEG C/min；
(7) molded samples are taken out after the completion of being sintered, target rim and surface are carefully ground using sand paper, by table
Face polishes smooth to obtain the target of preparation extension nanostructure；
(8) nanoporous template resistant to high temperature is used, foraminous die plate absorption is covered in monocrystal chip surface, monocrystal chip
For single crystalline Si substrate, Si/Pt substrate, monocrystalline Al2O3Substrate or monocrystalline SrTiO3One of substrate, nanostructure preparation use
Pulse laser deposition plating technology, background vacuum pressure are higher than 2 × 10-4Pa；
(9) substrate temperature when nano structure membrane is grown is 850 DEG C, the speed of rotation 1R/min of substrate, substrate and target
The distance between material is 10cm, and the target speed of rotation is 6R/min, and the power of pulse laser is 100mJ/cm2, frequency 2Hz,
Rate of temperature fall after nano structure membrane has been grown is 40 DEG C/min, and cooling air pressure is oxygen, and oxygen pressure is 0.8MPa；It removes resistance to
The nanoporous template of high temperature obtains hexad ferrite nano-structure array, and atmosphere when nano structure membrane is grown is flowing
Oxygen, oxygen pressure are 5Pa, flow rate 40sccm；
(10) the after annealing temperature of nano-structure array are as follows: 1250 DEG C, heating rate is 2 DEG C/min, rate of temperature fall 3
DEG C/min, after annealing atmosphere is flowing oxygen, and oxygen pressure is 5Pa, flow rate 40sccm.
The M type hexad ferrite (BaFe that embodiment 2 is prepared10.2Sc1.8O19, abbreviation BFSO) and extension nanostructure
Array sample is characterized:
(1) XRD characterization: taking extension BFSO nano-dot matrix sample and extension BFSO film to carry out, as a result as shown in Figure 1, outer
The X-ray diffraction peak (XRD) for prolonging BFSO nano-dot matrix sample is consistent with extension BFSO film, and surface BFSO nano-dot matrix is C-
The epitaxial growth of axis out-of-plane orientation.
(2) TEM Electronic Speculum: as shown in Figure 2, BFSO nano-dot matrix sample has regular periodic surface pattern.
(3) magnetism testing: from the figure 3, it may be seen that the coercivity of the outer hysteresis loop of the BFSO nano-dot matrix sample surface of preparation is very
It is small, it is almost the same with the coercivity and hysteresis loop shape of BFSO film reported in the literature, it was demonstrated that we are successfully prepared low
Coercitive multiferroic M type hexad ferrite BFSO extension nano-structure array sample.
Claims (6)
1. a kind of preparation method of extension hexad ferrite nano-dot matrix structure, it is characterised in that: include the following steps
(1) Ferrite Material in the present invention has molecular formula: AFe12-xMxO19, wherein A be in Ba element or Sr element at least
One kind, M are Sc element, x numberical range are as follows: 1.78 < x≤1.9.With high-purity BaCO3、SrCO3、Fe2O3,Sc2O3Powder is raw material,
By the atomic molar in molecular formula than proportion, it is put into after mixing raw material after weighing in ball mill and carries out ball milling；
(2) it is put into dryer and dries after the completion of ball milling, dryer temperature is 70-100 DEG C, and drying time is 30-50 minutes；
(3) raw material grind after drying is placed in crucible, is put into tube furnace and carries out preheating；Tube furnace is according to temperature ladder
Degree heating, heating rate are 2 DEG C/min, and calcined temperature is 800-1000 DEG C, and burn-in time is 17-24 hours, after pre-burning
Rate of temperature fall be 1-3 DEG C/min；
(4) 3-5 drop PET is instilled hand lapping 20-40 minutes after the completion of pre-burning, in pre-burning medicine powder and bonds glue, is ground again
Mill is not obviously bonded up to no caking phenomenon and with mortar wall；
(5) powder is poured into mold, pressurization 5-10MPa keeps 10-15min, and molded samples are taken out after decompression, observes sample
With the presence or absence of slight crack etc., if it exists slight crack then need to grind again as powder and again compacting until flawless；
(6) molded samples are put into sintering processes in tube furnace, tube furnace heats up according to temperature gradient, heating rate be 2 DEG C/
Min, sintering temperature are 1220 DEG C, and sintering time is 17-24 hours, and the rate of temperature fall after the completion of being sintered is 1-3 DEG C/min；
(7) molded samples are taken out after the completion of being sintered, target rim and surface are carefully ground using sand paper, surface is beaten
Ground smooth obtains the target of preparation extension nanostructure；
(8) nanoporous template resistant to high temperature is used, foraminous die plate absorption is covered in monocrystal chip surface, nanostructure preparation
Using pulse laser deposition plating technology, background vacuum pressure is higher than 2 × 10-4Pa；
(9) substrate temperature when nano structure membrane is grown is 650-850 DEG C, and the speed of rotation of substrate is 1-3R/min, substrate
The distance between target is 7-10cm, and the target speed of rotation is 6-10R/min, and the power of pulse laser is 10-100mJ/
cm2, frequency 2-10Hz, the rate of temperature fall after nano structure membrane has been grown is 15-40 DEG C/min, and cooling air pressure is oxygen,
Oxygen pressure is 15kPa-0.8MPa；Nanoporous template resistant to high temperature is removed, hexad ferrite nano-structure array is obtained；
(10) the after annealing temperature of nano-structure array are as follows: 1050-1250 DEG C, heating rate is 2-5 DEG C/min, and rate of temperature fall is
1-3℃/min。
2. the preparation method of extension hexad ferrite nano-dot matrix structure as described in claim 1, it is characterised in that: the step
Suddenly drum's speed of rotation is 200-300R/min in (1), and Ball-milling Time is 10-20 hours.
3. the preparation method of extension hexad ferrite nano-dot matrix structure as described in claim 1, it is characterised in that: the step
It suddenly is air or flowing oxygen atmosphere in the tube furnace in (3).
4. the preparation method of extension hexad ferrite nano-dot matrix structure as described in claim 1, it is characterised in that: the list
Brilliant substrate is single crystalline Si substrate, Si/Pt substrate, monocrystalline Al2O3Substrate or monocrystalline SrTiO3One of substrate.
5. the preparation method of extension hexad ferrite nano-dot matrix structure as described in claim 1, it is characterised in that: the step
Suddenly atmosphere when nano structure membrane is grown in (9) is flowing oxygen, and oxygen pressure is 5-25Pa, flow rate 15-40sccm.
6. the preparation method of extension hexad ferrite nano-dot matrix structure as described in claim 1, it is characterised in that: the step
Suddenly after annealing atmosphere is flowing oxygen in (10), and oxygen pressure is 5-30Pa, flow rate 15-40sccm.
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| CN110491771A (en) * | 2019-07-11 | 2019-11-22 | 华南理工大学 | The preparation method of metal oxide thin-film transistor and preparation method thereof and passivation layer |
| CN110581332A (en) * | 2019-08-23 | 2019-12-17 | 电子科技大学 | Self-biased millimeter wave circulator based on M-shaped hexagonal ferrite nanowire array |
| CN111020499A (en) * | 2019-12-06 | 2020-04-17 | 西安交通大学 | Preparation method of flexible microwave ferrite film |
| CN112939590A (en) * | 2021-03-12 | 2021-06-11 | 电子科技大学 | Hexahexaferrite material for X-band quasi-planar device and preparation method thereof |
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| CN110491771A (en) * | 2019-07-11 | 2019-11-22 | 华南理工大学 | The preparation method of metal oxide thin-film transistor and preparation method thereof and passivation layer |
| CN110581332A (en) * | 2019-08-23 | 2019-12-17 | 电子科技大学 | Self-biased millimeter wave circulator based on M-shaped hexagonal ferrite nanowire array |
| CN110581332B (en) * | 2019-08-23 | 2021-10-26 | 电子科技大学 | Self-biased millimeter wave circulator based on M-shaped hexagonal ferrite nanowire array |
| CN111020499A (en) * | 2019-12-06 | 2020-04-17 | 西安交通大学 | Preparation method of flexible microwave ferrite film |
| CN112939590A (en) * | 2021-03-12 | 2021-06-11 | 电子科技大学 | Hexahexaferrite material for X-band quasi-planar device and preparation method thereof |
| CN112939590B (en) * | 2021-03-12 | 2022-10-14 | 电子科技大学 | Hexahexaferrite material for X-band quasi-planar device and preparation method thereof |
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