CN106893976A - A kind of method for preparing MgO film as target with high-purity compact magnesia - Google Patents
A kind of method for preparing MgO film as target with high-purity compact magnesia Download PDFInfo
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- CN106893976A CN106893976A CN201710036803.6A CN201710036803A CN106893976A CN 106893976 A CN106893976 A CN 106893976A CN 201710036803 A CN201710036803 A CN 201710036803A CN 106893976 A CN106893976 A CN 106893976A
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- mgo film
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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
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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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
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of method for preparing MgO film as target with high-purity compact magnesia, comprise the following steps：(1) after magnesium oxide powder is ground, the powder after sieving is carried out isostatic cool pressing (CIP) shaping by sieving, pressed compact is obtained, pressed compact is carried out into pre-sintering first at 520 DEG C, intensification is vacuumized afterwards and is sintered, after the completion of sintering, high-purity compact magnesium oxide material is obtained；(2) with high-purity compact magnesium oxide material obtained in previous step as target, the growth of MgO film is carried out in the reative cell of magnetically controlled DC sputtering device, reaction completes to take out MgO film.Method of the present invention is target using high-purity compact magnesia, and the MgO film of preparation has good electrical and optical property, and thickness distribution is uniform, quality zero defect high.
Description
Technical field
The present invention relates to MgO film field, more particularly to one kind prepares MgO film by target of high-purity compact magnesia
Method.
Background technology
Magnetic random access memory (MRAM) is a kind of non-volatile computer memory technology, and the technology is from last century
Start development the nineties, surprising progress has been obtained at present.Basic mram memory cell includes two very thin insulators
Gap between separated trilamellar membrane structure, two pieces of pole plates is referred to as magnetic tunnel-junction (MTJ).The negative electrode of magnetic tunnel-junction separation layer
Using magnesia film more in the source.
The preparation method of conventional magnesia film has：Pulsed laser deposition, sputtering method and sol-gel process.Wherein
Pulsed laser deposition refers to the pole by the way that the high power pulsed laser Shu Huiju produced by excimer pulse laser is produced
High-temperature acts on target material surface so that target corrode produces high temperature, the plasma of high pressure, and these plasmas orientation occurs
Local expansion transmitting, deposits on substrate so as to form nano thin-film；The method has the advantages that to use scope wide, but also has
Film thickness is difficult to control to, the shortcomings of operating cost is larger.Sol-gel process refers to lead in the solution containing metallic compound
Crossing carries out decomposition, polymerization, and solution is become to be dispersed with the sol solutionses of metal oxide microparticle, afterwards sends out sol solutionses
Raw gel reaction, then by being heat-treated to gel after prepare the materials such as polycrystalline ceramics；The method cost is relatively low, but system
The more difficult control of standby film thickness.Sputtering method refers to the process of that target material is ejected and is deposited on substrate, including ion
Sputtering and magnetron sputtering, are to be attracted the gas ion with positive charge in plasma by the negative electrode below target, Xiang Qi
High-speed motion bombards target particle, because the part target particle that momentum transmission makes flies out, so as to be deposited into film.Wherein magnetic control
Sputtering is divided into：Radio-frequency magnetron sputter method, reactive magnetron sputtering method and direct current magnetron sputtering process.The target in magnetically controlled sputter method
Selection is the key for feeling film quality.Magnetron sputtering prepares magnesia film and typically uses two kinds of targets：Pure zirconia magnesium target
And Mg targets.
Chinese patent CN01133479.7 discloses a kind of MgO film preparation technology, and the invention uses multi-arc ion coating method,
With pure Mg as cathode target, anode is connected with vacuum chamber, and negative electrode and anode are connected on the negative pole of low pressure, high-current dc power supply respectively
And positive pole；Before shove charge first with HF acid cleaning matrix, vacuum is evacuated to 8 × 10-3~2.0 × 10-2Pa after shove charge, be passed through Ar gas with
H2, increases 500~700V of bias, and matrix surface is bombarded using glow discharge, and bombardment time is 3~5min, uses O2Make
Reacting gas, protective gas is made with Ar gas, and oxygen flow is 160~270Sccm, and the copper air guide pipe end of Ar gas is made into circle
Shape, its size is more bigger than Mg target, by its close Mg target, and O2The use air guide mouth of pipe then near matrix, with contact short circuit method striking
Plating, arc current is 20~40A, and arc voltage is 15V~40V, and operating pressure is 2.0~8.0 × 10-1Pa.The invention economy,
Nuisanceless, deposition velocity is fast, can at low temperature deposit and consistency is high, but operating process is complex.
The content of the invention
It is an object of the invention to provide a kind of method for preparing MgO film as target with high-purity compact magnesia, the method
The use of high-purity compact magnesia is target, the MgO film of preparation has good electrical and optical property, and thickness distribution is uniform, matter
Measure zero defect high.
To achieve the above object, the present invention uses following technical scheme：
A kind of method for preparing MgO film as target with high-purity compact magnesia, comprises the following steps：
(1) by magnesium oxide powder addition marble mill, mill ball is added, is ground with the speed rotation of 180-280rpm
Mill, every behind 30min switching-over grindings direction, grinding 12-16h, powder takes out, sieving, the powder after sieving is carried out cold etc. quiet
Pressure (CIP) shaping, is obtained pressed compact, and pressed compact is carried out into pre-sintering first at 520 DEG C, intensification is vacuumized afterwards and is sintered, and sinters
After the completion of, high-purity compact magnesium oxide material is obtained；
(2) with high-purity compact magnesium oxide material obtained in previous step as target, in the reaction of magnetically controlled DC sputtering device
The substrate for cleaning is put into room, after being evacuated to vacuum ＜ 1Pa, heating substrate is passed through Ar gas to 450-550 DEG C, controls
Reaction intraventricular pressure is by force 1-3Pa, and the growth of MgO film is carried out under 90-110W power, and room temperature is down to after the completion of reaction, is passed through
Air, takes out MgO film.
Preferably, the raw material magnesium oxide powder is that purity is higher than 99.99%, and impurity element total content is less than 100ppm.
Preferably, mill ball be zirconium oxide abrasive ball, be diameter 3mm and diameter 1mm etc. mass mixing thing.
Preferably, mill ball and the input amount mass ratio of magnesium oxide powder are 1:(2-4).
Preferably, sieving in step (1), mesh size is 300-400 mesh.
Preferably, temperature control is in the sintering process：Below 600 DEG C, heating rate is 20 DEG C/min, is exceeded
Heating rate is 65 DEG C/min after 600 DEG C, and after rising to 1400 DEG C, keeping temperature 10min drops according to the speed of 30 DEG C/min afterwards
Low temperature is to normal temperature.
Preferably, the substrate is silicon or silica.
The cleaning process of wherein substrate is：Substrate is carried out into ultrasonic cleaning 2-4h with deionized water first, is put afterwards
It is placed in alcohol and is cleaned by ultrasonic 45-90min with continuation in the mixed liquor of petroleum ether, after being flushed three times with deionized water afterwards, is putting
Enter and be cleaned by ultrasonic 30-45min, vacuumizing and drying in deionized water.
The invention has the advantages that, it is target to use the high-purity compact magnesia for voluntarily preparing, using DC magnetic
Control sputtering method prepares MgO film.Prepare during magnesium oxide material, magnesium oxide powder is fully ground first, using row
Magnesia is ground to form particle dispersion powder high by star ball-milling method, improves particle internal distortions energy；Using cold isostatic pressing
Shaping, improves its density, and the consistency of the material that raising is sintered out, particle size is more tiny homogeneous；Suitable sintering is true
Air atmosphere can effectively avoid the too high caused MgO accelerated decompositions of vacuum, can also promote densification.Using the MgO materials
Expect to be MgO film prepared by target, thickness has a good homogeneity, purity zero defect high, with good electricity, optical
Energy.
Specific embodiment
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of method for preparing MgO film as target with high-purity compact magnesia, comprises the following steps：
(1) it is higher than 99.99% by purity, magnesium oxide powder of the impurity element total content less than 100ppm adds marble to grind
In grinder, mill ball is added, with the speed spin finishing of 180rpm, every 30min switching-over grindings direction, after grinding 12h, powder
Take out, sieving, mesh size is 300 mesh, the powder after sieving is carried out into isostatic cool pressing (CIP) shaping, pressed compact is obtained, pressed compact is existed
520 DEG C carry out pre-sintering first, intensification is vacuumized afterwards and is sintered, and after the completion of sintering, high-purity compact magnesium oxide material are obtained；
(2) with high-purity compact magnesium oxide material obtained in previous step as target, in the reaction of magnetically controlled DC sputtering device
The silicon dioxide substrates cleaned are put into room, after being evacuated to vacuum ＜ 1Pa, heating substrate is passed through Ar gas to 450 DEG C,
Control reaction intraventricular pressure is by force 1Pa, and the growth of MgO film is carried out under 92W power, and room temperature is down to after the completion of reaction, is passed through big
Gas, takes out MgO film.
Mill ball be zirconium oxide abrasive ball, be diameter 3mm and diameter 1mm etc. mass mixing thing；Mill ball and magnesia
The input amount mass ratio of powder is 1:2.
Temperature control is in sintering process：Below 600 DEG C, heating rate be 20 DEG C/min, more than 600 DEG C after heat up speed
Rate is 65 DEG C/min, after rising to 1400 DEG C, keeping temperature 10min, afterwards according to the rate reduction temperature of 30 DEG C/min to normal temperature.
The cleaning process of wherein substrate is：Substrate is carried out into ultrasonic cleaning 2h with deionized water first, is placed afterwards
Continue to be cleaned by ultrasonic 90min in the mixed liquor of alcohol and petroleum ether, after being flushed three times with deionized water afterwards, be put into from
It is cleaned by ultrasonic 30min, vacuumizing and drying in sub- water.
The purity of wherein obtained high-purity compact magnesium oxide material is 99.99%, and consistency is 98.64%；Obtained MgO
Film dense uniform, caliper uniformity is good.
Embodiment 2
A kind of method for preparing MgO film as target with high-purity compact magnesia, comprises the following steps：
(1) it is higher than 99.99% by purity, magnesium oxide powder of the impurity element total content less than 100ppm adds marble to grind
In grinder, mill ball is added, with the speed spin finishing of 280rpm, every 30min switching-over grindings direction, after grinding 16h, powder
Take out, sieving, mesh size is 400 mesh, the powder after sieving is carried out into isostatic cool pressing (CIP) shaping, pressed compact is obtained, pressed compact is existed
520 DEG C carry out pre-sintering first, intensification is vacuumized afterwards and is sintered, and after the completion of sintering, high-purity compact magnesium oxide material are obtained；
(2) with high-purity compact magnesium oxide material obtained in previous step as target, in the reaction of magnetically controlled DC sputtering device
The silicon substrate for cleaning is put into room, after being evacuated to vacuum ＜ 1Pa, heating substrate is passed through Ar gas to 550 DEG C, and control is anti-
It is 3Pa to answer indoor pressure, and the growth of MgO film is carried out under 110W power, and room temperature is down to after the completion of reaction, is passed through air, is taken
Go out MgO film.
Mill ball be zirconium oxide abrasive ball, be diameter 3mm and diameter 1mm etc. mass mixing thing；Mill ball and magnesia
The input amount mass ratio of powder is 1:4.
Temperature control is in sintering process：Below 600 DEG C, heating rate be 20 DEG C/min, more than 600 DEG C after heat up speed
Rate is 65 DEG C/min, after rising to 1400 DEG C, keeping temperature 10min, afterwards according to the rate reduction temperature of 30 DEG C/min to normal temperature.
The cleaning process of wherein substrate is：Substrate is carried out into ultrasonic cleaning 4h with deionized water first, is placed afterwards
Continue to be cleaned by ultrasonic 90min in the mixed liquor of alcohol and petroleum ether, after being flushed three times with deionized water afterwards, be put into from
It is cleaned by ultrasonic 45min, vacuumizing and drying in sub- water.
The purity of wherein obtained high-purity compact magnesium oxide material is 99.99%, and consistency is 99.23%；Obtained MgO
Film dense uniform, caliper uniformity is good.
Embodiment 3
A kind of method for preparing MgO film as target with high-purity compact magnesia, comprises the following steps：
(1) it is higher than 99.99% by purity, magnesium oxide powder of the impurity element total content less than 100ppm adds marble to grind
In grinder, mill ball is added, with the speed spin finishing of 280rpm, every 30min switching-over grindings direction, after grinding 12h, powder
Take out, sieving, mesh size is 400 mesh, the powder after sieving is carried out into isostatic cool pressing (CIP) shaping, pressed compact is obtained, pressed compact is existed
520 DEG C carry out pre-sintering first, intensification is vacuumized afterwards and is sintered, and after the completion of sintering, high-purity compact magnesium oxide material are obtained；
(2) with high-purity compact magnesium oxide material obtained in previous step as target, in the reaction of magnetically controlled DC sputtering device
The silicon dioxide substrates cleaned are put into room, after being evacuated to vacuum ＜ 1Pa, heating substrate is passed through Ar gas to 450 DEG C,
Control reaction intraventricular pressure is by force 3Pa, and the growth of MgO film is carried out under 90W power, and room temperature is down to after the completion of reaction, is passed through big
Gas, takes out MgO film.
Mill ball be zirconium oxide abrasive ball, be diameter 3mm and diameter 1mm etc. mass mixing thing；Mill ball and magnesia
The input amount mass ratio of powder is 1:4.
Temperature control is in sintering process：Below 600 DEG C, heating rate be 20 DEG C/min, more than 600 DEG C after heat up speed
Rate is 65 DEG C/min, after rising to 1400 DEG C, keeping temperature 10min, afterwards according to the rate reduction temperature of 30 DEG C/min to normal temperature.
The cleaning process of wherein substrate is：Substrate is carried out into ultrasonic cleaning 4h with deionized water first, is placed afterwards
Continue to be cleaned by ultrasonic 45min in the mixed liquor of alcohol and petroleum ether, after being flushed three times with deionized water afterwards, be put into from
It is cleaned by ultrasonic 45min, vacuumizing and drying in sub- water.
The purity of wherein obtained high-purity compact magnesium oxide material is 99.99%, and consistency is 98.77%；Obtained MgO
Film dense uniform, caliper uniformity is good.
Embodiment 4
A kind of method for preparing MgO film as target with high-purity compact magnesia, comprises the following steps：
(1) it is higher than 99.99% by purity, magnesium oxide powder of the impurity element total content less than 100ppm adds marble to grind
In grinder, mill ball is added, with the speed spin finishing of 200rpm, every 30min switching-over grindings direction, after grinding 14h, powder
Take out, sieving, mesh size is 300 mesh, the powder after sieving is carried out into isostatic cool pressing (CIP) shaping, pressed compact is obtained, pressed compact is existed
520 DEG C carry out pre-sintering first, intensification is vacuumized afterwards and is sintered, and after the completion of sintering, high-purity compact magnesium oxide material are obtained；
(2) with high-purity compact magnesium oxide material obtained in previous step as target, in the reaction of magnetically controlled DC sputtering device
The silicon substrate for cleaning is put into room, after being evacuated to vacuum ＜ 1Pa, heating substrate is passed through Ar gas to 500 DEG C, and control is anti-
It is 2Pa to answer indoor pressure, and the growth of MgO film is carried out under 100W power, and room temperature is down to after the completion of reaction, is passed through air, is taken
Go out MgO film.
Mill ball be zirconium oxide abrasive ball, be diameter 3mm and diameter 1mm etc. mass mixing thing；Mill ball and magnesia
The input amount mass ratio of powder is 1:3.
Temperature control is in sintering process：Below 600 DEG C, heating rate be 20 DEG C/min, more than 600 DEG C after heat up speed
Rate is 65 DEG C/min, after rising to 1400 DEG C, keeping temperature 10min, afterwards according to the rate reduction temperature of 30 DEG C/min to normal temperature.
The cleaning process of wherein substrate is：Substrate is carried out into ultrasonic cleaning 3h with deionized water first, is placed afterwards
Continue to be cleaned by ultrasonic 60min in the mixed liquor of alcohol and petroleum ether, after being flushed three times with deionized water afterwards, be put into from
It is cleaned by ultrasonic 40min, vacuumizing and drying in sub- water.
The purity of wherein obtained high-purity compact magnesium oxide material is 99.99%, and consistency is 99.09%；Obtained MgO
Film dense uniform, caliper uniformity is good.
Claims (7)
1. a kind of method for preparing MgO film as target with high-purity compact magnesia, it is characterised in that comprise the following steps：
(1) by magnesium oxide powder addition marble mill, mill ball is added, with the speed spin finishing of 180-280rpm,
Every behind 30min switching-over grindings direction, grinding 12-16h, powder is taken out, sieving, and the powder after sieving is carried out into isostatic cool pressing
(CIP) it is molded, pressed compact is obtained, pressed compact is carried out into pre-sintering first at 520 DEG C, intensification is vacuumized afterwards and is sintered, has sintered
Cheng Hou, is obtained high-purity compact magnesium oxide material；
(2) with high-purity compact magnesium oxide material obtained in previous step as target, in the reative cell of magnetically controlled DC sputtering device
The substrate for cleaning is put into, after being evacuated to vacuum ＜ 1Pa, heating substrate is passed through Ar gas, control reaction to 450-550 DEG C
Indoor pressure is 1-3Pa, and the growth of MgO film is carried out under 90-110W power, and room temperature is down to after the completion of reaction, is passed through air,
Take out MgO film.
2. the method for preparing MgO film as target with high-purity compact magnesia according to claim 1, it is characterised in that：
The raw material magnesium oxide powder is that purity is higher than 99.99%, and impurity element total content is less than 100ppm.
3. the method for preparing MgO film as target with high-purity compact magnesia according to claim 1, it is characterised in that：
Mill ball be zirconium oxide abrasive ball, be diameter 3mm and diameter 1mm etc. mass mixing thing.
4. the method for preparing MgO film as target with high-purity compact magnesia according to claim 1, it is characterised in that：
Mill ball is 1 with the input amount mass ratio of magnesium oxide powder:(2-4).
5. the method for preparing MgO film as target with high-purity compact magnesia according to claim 1, it is characterised in that：
Sieving in step (1), mesh size is 300-400 mesh.
6. the method for preparing MgO film as target with high-purity compact magnesia according to claim 1, it is characterised in that：
Temperature control is in the sintering process：Below 600 DEG C, heating rate be 20 DEG C/min, more than 600 DEG C after heating rate be
65 DEG C/min, after rising to 1400 DEG C, keeping temperature 10min, afterwards according to the rate reduction temperature of 30 DEG C/min to normal temperature.
7. the method for preparing MgO film as target with high-purity compact magnesia according to claim 1, it is characterised in that：
The substrate is silicon or silica.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116874284A (en) * | 2023-07-13 | 2023-10-13 | 宁波江丰电子材料股份有限公司 | Preparation method of magnesium oxide target |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10130828A (en) * | 1996-10-31 | 1998-05-19 | Mitsubishi Materials Corp | Mgo target and its production |
| JPH10130827A (en) * | 1996-10-28 | 1998-05-19 | Mitsubishi Materials Corp | Mgo target and its production |
| CN103415486A (en) * | 2011-03-24 | 2013-11-27 | 达泰豪化学工业株式会社 | Process for producing sintered magnesium oxide material |
-
2017
- 2017-01-18 CN CN201710036803.6A patent/CN106893976A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10130827A (en) * | 1996-10-28 | 1998-05-19 | Mitsubishi Materials Corp | Mgo target and its production |
| JPH10130828A (en) * | 1996-10-31 | 1998-05-19 | Mitsubishi Materials Corp | Mgo target and its production |
| CN103415486A (en) * | 2011-03-24 | 2013-11-27 | 达泰豪化学工业株式会社 | Process for producing sintered magnesium oxide material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116874284A (en) * | 2023-07-13 | 2023-10-13 | 宁波江丰电子材料股份有限公司 | Preparation method of magnesium oxide target |
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