CN116253560B - Alumina target and preparation method thereof - Google Patents
Alumina target and preparation method thereof Download PDFInfo
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- CN116253560B CN116253560B CN202211615768.0A CN202211615768A CN116253560B CN 116253560 B CN116253560 B CN 116253560B CN 202211615768 A CN202211615768 A CN 202211615768A CN 116253560 B CN116253560 B CN 116253560B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 86
- 238000005245 sintering Methods 0.000 claims abstract description 53
- 239000004576 sand Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 15
- 238000000748 compression moulding Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 17
- 239000013077 target material Substances 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 238000009461 vacuum packaging Methods 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 235000015895 biscuits Nutrition 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000004321 preservation Methods 0.000 description 7
- 230000000630 rising effect Effects 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000011268 mixed slurry Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- 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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- 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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- 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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Abstract
The application relates to the technical field of oxide target production, and discloses an alumina target and a preparation method thereof, wherein the alumina target comprises the following steps: preparing alumina powder; putting the alumina powder into a mould for compression molding to obtain an alumina blank; performing cold isostatic pressing treatment on the alumina blank to obtain a high-density alumina blank; paving a layer of sintered alumina sand on a sintering bearing plate in an atmospheric sintering furnace under the air atmosphere, placing a high-density alumina blank on the upper layer of the alumina sand, heating to 1000 ℃ at the heating rate of 0.5-1 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process; heating to 1000 deg.C, maintaining for 2-4 hr, heating to 1500-1600 deg.C at a rate of 0.01-0.3 deg.C/min, and maintaining at 30-200 deg.C for 2-10 hr during heating; the target prepared by the preparation method has the density of 3.97g/cm 3, and the maximum size of the target can reach 1.5 multiplied by 1.0m, so that the upper limit of the size of the target is greatly improved; in addition, an alumina target is also disclosed.
Description
Technical Field
The application relates to the technical field of oxide target production, in particular to an alumina target and a preparation method thereof.
Background
The development of the semiconductor technology level, the size of the device is gradually miniaturized, the requirements on film materials are higher and higher, and the Al 2O3 film is widely applied as the film with high dielectric constant, high band gap and high light transmittance. The Al 2O3 film is prepared by adopting an atomic layer deposition technology, the uniformity and the quality of the film are high, and a magnetron sputtering method is generally adopted in the preparation process of the Al 2O3 film, wherein the working principle of the magnetron sputtering is that electrons collide with argon atoms in the process of flying to a substrate under the action of an electric field E, so that Ar positive ions and new electrons are generated by ionization of the electrons; the new electrons fly to the substrate, ar ions fly to the cathode target in an accelerating way under the action of an electric field, and bombard the surface of the target with high energy, so that the target material is sputtered. In the sputtering particles, neutral target atoms or molecules are deposited on a substrate to form a film, so that the quality of the alumina target is critical to the preparation of the Al 2O3 film, for example, the density of the target is not high, the adsorption is not easy to occur when the density of the target is low, gaps are not formed, the back target is easy to fall off, and when the density of the target is high, the air hole content in the target solid is reduced, the performance of the sputtering film is improved, and meanwhile, the thermal stress in the sputtering process can be better borne by the target due to the improvement of the density of the target.
Meanwhile, in the actual production process of the target, in the prior art, the high-density target can be prepared by sintering in a vacuum furnace, for example, in CN101985735A, an alumina biscuit is heated to 1800 ℃ in the vacuum furnace with the vacuum degree higher than 2X 10 -3 Pa for sintering, and then the alumina target with the relative density of about 95% is obtained by sintering in a tubular furnace.
Chinese patent 202211074687.4 discloses an alumina target material and a preparation method and application thereof, and the preparation method comprises the following steps:
(1) Ball milling to mix alumina with grinding aid to obtain ball milling alumina;
(2) Ball-milling alumina obtained in the step (1) is subjected to first die filling and compaction, and is taken out and then is kept stand to obtain alumina blanks;
(3) Sequentially carrying out vacuum hot-pressing sintering and atmosphere sintering on the alumina blank obtained in the step (2) to obtain an alumina target blank;
(4) Machining the alumina target blank obtained in the step (3) to obtain the alumina target material; the vacuum hot-pressed sintering in the step (3) comprises a first heat treatment, a second heat treatment and a hot pressing treatment which are sequentially carried out.
According to the method, spherical powder is obtained by ball milling of alumina raw materials, a sintering process combining vacuum hot-pressing sintering and atmosphere sintering is adopted, reasonable sintering process parameters are matched, and the prepared alumina target has higher compactness and purity, but the method is focused on improving the compactness and purity of the target, but does not take excessive consideration on the improvement of the size of the target.
Chinese patent 202011324764.8 discloses a method for preparing an alumina target, comprising the steps of: (1) Mixing target raw materials, and ball milling to obtain mixed slurry, wherein the target raw materials comprise alumina powder, a binder and water;
(2) Spray drying the mixed slurry obtained in the step (1) to obtain mixed powder particles;
(3) Placing the mixture powder particles obtained in the step (2) into a die for pressing to obtain a biscuit, and then carrying out cold isostatic pressing treatment on the biscuit;
(4) Heating the biscuit subjected to cold isostatic pressing treatment to degreasing and sintering;
(5) Introducing oxygen, heating and sintering, and cooling and sintering;
(6) Heating and sintering to obtain the alumina target; the heating sintering in the step (5) is staged sintering; the temperature-rising sintering in the step (5) is divided into two-stage sintering, firstly, the temperature is raised to 1000-1300 ℃ at the speed of 0.1-0.5 ℃/min, the temperature is kept for 1-4h, then the temperature is raised to 1500-1550 ℃ at the speed of 0.1-0.5 ℃/min, and the temperature is kept for 4-8h;
the cooling and sintering treatment in the step (5) is as follows: cooling to 1200-1300 ℃ at the speed of 0.1-0.5 ℃/min, and preserving heat for 1-2h;
the heating sintering treatment in the step (6) is as follows: heating to 1550-1600 ℃ at the speed of 0.1-0.5 ℃/min, and preserving heat for 1-4h.
The target prepared by the method has higher relative density, the size of the target is improved, and the specification of the method is observed, so that the size of the target is improved to 1m multiplied by 1m, and the production efficiency is greatly improved in actual production.
The application solves the problems that: how to develop a preparation method of an alumina target, the size of the target can be continuously improved and the production efficiency can be improved on the premise of ensuring that the prepared target has high density and high yield.
Disclosure of Invention
The application aims to develop a preparation method of an alumina target, and the target prepared by the preparation method has the density of at least 3.97g/cm 3 and the maximum size of 1.5 multiplied by 1.5m, and the method greatly improves the upper limit of the size of the target on the premise of ensuring the density and the production yield of the target, so that the production efficiency of the target in the actual production process is improved.
The application is not specifically described: nM represents nanomole/liter, μM represents micromoles/liter, mM represents millimoles/liter, and M represents moles/liter;
the preparation method of the alumina target is characterized by comprising the following steps:
Step 1: preparing alumina powder;
Step 2: putting the alumina powder prepared in the step 1 into a die for compression molding to prepare an alumina blank;
Step 3: performing cold isostatic pressing treatment on the alumina blank obtained in the step 2to obtain a high-density alumina blank;
step 4: sintering the high-density alumina blank body obtained in the step 3 at a high temperature to obtain an alumina target material;
the step 4 specifically comprises the following steps: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing the high-density alumina blank body prepared in the step 3 on the alumina sand, heating to 1000 ℃ at a heating rate of 0.5-1 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process;
Heating to 1000 ℃ and preserving heat for 2-4h, then heating to 1500-1600 ℃ at the speed of 0.01-0.3 ℃/min, and preserving heat for 2-10h at the temperature of 30-200 ℃ in the heating process;
Step 4 is carried out under an air atmosphere.
More preferably, the step 4 specifically comprises:
Paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing the high-density alumina blank body prepared in the step 3 on the alumina sand, heating to 1000 ℃ at a heating rate of 0.5-1 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process;
Heating to 1000 ℃ and preserving heat for 2-4h, then heating to 1500-1600 ℃ at the speed of 0.01-0.3 ℃/min, and preserving heat for 2-10h at the temperature of 30-200 ℃ in the heating process;
and the temperature rising rate is reduced to 0.005-0.1 ℃/min after the temperature rises to 1300 ℃.
It should be noted and understood that the purity of the alumina raw material is not excessively limited, and the purity of the alumina raw material used in the present application is 4N, i.e. the purity of the alumina raw material is 99.99%, because the purity of the alumina raw material is not substantially affected by the purity of the alumina raw material, and the reason for selecting the alumina raw material with the purity is that the purity requirement of the product is high, and the purity of the alumina raw material can only affect the purity of the product, and the purity of the product is proportional to the purity of the alumina, which is also common knowledge of those skilled in the art.
Preferably, the step 1 specifically includes: adding an alumina raw material into a sand mill, wherein the diameter of a zirconium ball used in the sand milling process is 0.3-0.5mm;
And adding 5-10% of polyvinyl alcohol solution relative to the content of the alumina raw material into a sand mill while adding the alumina raw material, wherein the content of polyvinyl alcohol in the polyvinyl alcohol solution is 10-15%, and performing spray drying after finishing sanding, wherein the inlet temperature is 180-200 ℃, the outlet is 70-100 ℃, so as to obtain the alumina powder with D90<0.5 um.
Preferably, the step 2 specifically includes: loading the alumina powder prepared in the step 1 into a die, setting the pressure to be more than or equal to 16000KN for mechanical pressing, polishing corners of a blank body after mechanical pressing, and then vacuum packaging;
The corner radius R of the corner polishing is 0.5-1mm.
Preferably, the step 3 specifically includes: and (3) carrying out cold isostatic pressing on the packaged alumina blank obtained in the step (2) under the pressure of 200-300 MPa at the pressure increasing rate of 10-20 MPa/min for 5-10min, then reducing the pressure to 0MPa at the pressure reducing rate of 30-50MPa/min, and in the pressure reducing process, maintaining the pressure and standing for 1min every time the pressure is reduced, thereby obtaining the alumina blank with high density.
Preferably, the step 4 specifically includes: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing the alumina blank body prepared in the step 3 on the alumina sand, heating to 1000 ℃ at a heating rate of 0.6-0.8 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process;
Heating to 1000 deg.C, maintaining for 2-4 hr, heating to 1550-1600 deg.C at a rate of 0.05-0.2 deg.C/min, and maintaining at 50-100deg.C for 2-10 hr during heating;
Step 4 is carried out under an air atmosphere.
More preferably, the step 4 specifically comprises: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing the alumina blank body prepared in the step 3 on the alumina sand, heating to 1000 ℃ at a heating rate of 0.6-0.8 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process;
heating to 1000 ℃ and preserving heat for 2-4h, then heating to 1550-1600 ℃ at the speed of 0.05-0.2 ℃/min, and preserving heat for 2-10h at the temperature of 50-200 ℃ in the heating process;
and the temperature rising rate is reduced to 0.005-0.1 ℃/min after the temperature rises to 1300 ℃.
In practical application, in step 4, after heating to 1000 ℃ and maintaining the temperature for 2-4 hours, the temperature is further raised to an end point temperature at a rate of 0.05-0.2 ℃/min, wherein the end point temperature comprises, but is not limited to 1550 ℃, 1560 ℃, 1570 ℃, 1580 ℃, 1590 ℃, 1600 ℃.
Preferably, the dimensions of the mould in step 1 are 500-1500mm x 200-1000mm, and the pressure during the mechanical pressing is 16000KN-25000KN.
Preferably, in step 2, the alumina powder prepared in step 1 and having a bulk density of 1.0-1.2g/cm 3 and a moisture content of 0.8-1.2% is selected and put into a mold for molding.
Preferably, in the step 4, the alumina blank which is prepared in the step 3 and has the density of more than 2.2g/cm 3 is placed on the upper layer of alumina sand, the temperature is raised to 1000 ℃ at the heating rate of 0.6-0.8 ℃/min, and the temperature is kept for 2-4 hours at 200 ℃ per rise; heating to 1000 deg.C, maintaining the temperature, heating to 1550-1600 deg.C at the rate of 0.05-0.2 deg.C/min, and maintaining the temperature at 30-200 deg.C for 6-10 hr;
Step 4 is carried out under an air atmosphere.
In addition, the application also discloses an alumina target material, which is prepared by adopting the preparation method of the alumina target material.
Preferably, the density of the alumina target is at least 3.97g/cm 3, and the size of the alumina target is 500-1500mm×200-1000mm.
The beneficial effects of the application are as follows: the target prepared by the preparation method has the density of at least 3.97g/cm 3, and the maximum size of the target can reach 1.5 multiplied by 1.0m, and the method greatly improves the upper limit of the size of the target on the premise of ensuring the density and the production yield of the target, so that the production efficiency of the target in the actual production process is improved.
Detailed Description
The present application will be described more fully hereinafter with reference to the accompanying drawings, in which specific conditions, either conventional or manufacturer-suggested, are not explicitly stated. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Step 1: adding an alumina raw material with the purity of 99.99% into a sand mill, adding a PVA (polyvinyl alcohol) solution with the purity of 5%, adopting zirconium balls with the diameter of 0.3mm, sanding the alumina until the particle diameter D90 of the alumina is less than 0.5um, and performing spray drying after finishing sanding, wherein the inlet temperature is 180 ℃ and the outlet temperature is 100 ℃ to obtain the prepared alumina powder;
Step 2: putting alumina powder into a mould with the size of 1000mm multiplied by 1000mm, setting the pressure of 20000KN for mechanical pressing for 8 minutes, polishing corners of the pressed blank, wherein the R of the polished corners is 0.8mm, and carrying out vacuum packaging after polishing to obtain an alumina blank;
Step 3: and (3) carrying out cold isostatic pressing on the packaged alumina blank, wherein the pressure increasing rate is 15MPa, after the pressure is increased to 300MPa, maintaining the pressure for 10min, then reducing the pressure, the pressure rate is 30MPa/min, reducing the pressure to 0MPa, and in the pressure reducing process, maintaining the pressure for 1 min every 50MPa, and obtaining the high-density alumina blank after the pressure reduction is completed.
Step 4: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing a high-density alumina blank on the alumina sand, heating to 1000 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 4 hours at every 200 ℃ in the heating process of 0-1000 ℃;
after the temperature is kept at 1000 ℃ for 4 hours, the temperature is raised to 1550 ℃ at a heating rate of 0.2 ℃/min, and in the heating process of 1000-1550 ℃, the temperature is kept for 4 hours after the temperature is raised by 100 ℃; when the temperature is increased to 1550 ℃, preserving heat for 10 hours;
at the same time, step 4 is carried out under an air atmosphere.
Example 2
Substantially the same as in example 1, except that step 4 specifically comprises: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing a high-density alumina blank on the alumina sand, heating to 1000 ℃ at a heating rate of 1 ℃/min, and keeping the temperature for 4 hours at 200 ℃ when the temperature is raised in the heating process of 0-1000 ℃;
After the heat preservation is carried out for 4 hours at 1000 ℃, the temperature is raised to 1600 ℃ at a heating rate of 0.3 ℃/min, and in the heating process of 1000-1600 ℃, the heat preservation is carried out for 4 hours when the temperature is raised to 1600 ℃ every 100 ℃ and the temperature is kept for 10 hours;
at the same time, step 4 is carried out under an air atmosphere.
Example 3
Substantially the same as in example 1, except that step 4 specifically comprises: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing a high-density alumina blank on the alumina sand, heating to 1000 ℃ at a heating rate of 0.5 ℃/min, and preserving heat for 4 hours at every 200 ℃ in the heating process of 0-1000 ℃;
After the heat preservation is carried out for 4 hours at 1000 ℃, the temperature is raised to 1500 ℃ at a heating rate of 0.05 ℃/min, and in the heating process of 1000-1400 ℃, the heat preservation is carried out for 4 hours when the temperature is raised to 1500 ℃ every 100 ℃ and the temperature is kept for 10 hours;
at the same time, step 4 is carried out under an air atmosphere.
Example 4
Substantially the same as in example 1, except that the die used in step2 was 1500mm by 1000mm in size and 23000KN in pressure.
Example 5
Substantially the same as in example 1, except that the die used in step 2 was 500mm×200mm in size and 16000KN in pressure.
Example 6
Substantially the same as in example 1, except that the die used in step2 was 1500mm by 1000mm in size and 25000KN in pressure;
The step4 is specifically as follows: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing a high-density alumina blank on the alumina sand, heating to 1000 ℃ at a heating rate of 0.7 ℃/min, and preserving heat for 4 hours at every 200 ℃ in the heating process of 0-1000 ℃;
After the heat preservation at 1000 ℃ for 4 hours, heating to 1550 ℃ at a heating rate of 0.2 ℃/min, and in the heating process of 1000-1550 ℃, keeping the temperature for 8 hours when the temperature is raised to 1550 ℃ every 100 ℃ and keeping the temperature for 10 hours;
meanwhile, step 4 is carried out under an air atmosphere.
Example 7
Substantially the same as in example 1, except that step 3 specifically comprises: and (3) carrying out cold isostatic pressing on the packaged alumina blank obtained in the step (2) at a pressure increasing rate of 10MPa/min to 200MPa, then reducing the pressure to 0MPa at a pressure reducing rate of 50MPa/min, and maintaining the pressure and standing for 1min every time the pressure is reduced by 50MPa in the pressure reducing process, so as to obtain the alumina blank with high density.
Example 8
Substantially the same as in example 1, except that a layer of sintered alumina sand was laid on a setter plate in an atmospheric sintering furnace, a high-density alumina green body was placed on the alumina sand, and the temperature was raised to 1000 c at a temperature-raising rate of 0.7 c/min, and during the temperature-raising process of 0-1000 c, heat was kept for 4 hours at 200 c each time;
after the heat preservation at 1000 ℃ for 4 hours, heating to 1300 ℃ at a heating rate of 0.2 ℃/min, and in the heating process of 1000-1300 ℃, keeping the temperature for 4 hours when the temperature is raised by 100 ℃, keeping the temperature for 4 hours after the heat preservation at 1300 ℃ for 4 hours, keeping the temperature for 5 hours when the temperature is raised by 50 ℃ in the heating process until the temperature is raised to 1550 ℃ and when the temperature is raised to 1550 ℃, keeping the temperature for 10 hours;
meanwhile, step 4 is carried out under an air atmosphere.
Example 9
Substantially the same as in example 1, except that in step 2, the alumina powder obtained in step 1 and having a bulk density of 1.1g/cm 3 and a moisture content of 1.0% was charged into a mold for molding.
Example 10
Substantially the same as in example 1, except that in step 4, an alumina target was prepared by selecting an alumina green body having a density of more than 2.2g/cm 3 obtained in step 3.
Comparative example 1
Substantially the same as in example 1, except that step 4 specifically comprises: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing a high-density alumina blank on the alumina sand, heating to 1550 ℃ at a heating rate of 0.5 ℃/min, and keeping the temperature for 10h when the temperature is raised to 1550 ℃ every 200 ℃ in the heating process of 0-1550 ℃;
meanwhile, step 4 is carried out under an air atmosphere.
Comparative example 2
Substantially the same as in example 1, except that step 3 specifically comprises: and (3) carrying out cold isostatic pressing on the packaged alumina blank, wherein the pressure increasing rate is 10MPa/min, after the pressure is increased to 300MPa, maintaining the pressure for 10min, then reducing the pressure, and reducing the pressure rate to 30MPa/min until the pressure is reduced to the standard atmospheric pressure, and ending the cold isostatic pressing to obtain the high-density alumina blank.
Comparative example 3
(1) Weighing a certain amount of alumina powder, adding 5% of binder, 1% of dispersing agent and pure water, ball milling for 4 hours to obtain mixed slurry with solid content of 60%, and checking that the mixed slurry D50 is less than 0.5 mu m and the half-peak width is less than 0.5;
(2) Spray drying the mixed slurry obtained in the step (1) to obtain mixture powder particles with the granularity less than 200 microns, wherein the spray drying temperature is 250 ℃, and the feeding speed is 700mL/min;
(3) Placing the mixture powder particles obtained in the step (2) into a die with the diameter of 1.5mx1.0m, pressing under 40MPa to obtain a biscuit, and carrying out cold isostatic pressing treatment on the biscuit under 400MPa, wherein the pressure rising rate of the cold isostatic pressing treatment is 10MPa/min, and the pressure maintaining time is 20min;
(4) Placing the biscuit obtained in the step (3) through cold isostatic pressing treatment into a sintering furnace, heating to 400 ℃ at the speed of 0.2 ℃/min for degreasing and sintering, keeping the temperature for 2 hours, introducing oxygen, heating to 1300 ℃ at the speed of 0.4 ℃/min, keeping the temperature for 2 hours, continuously heating to 1530 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 4 hours, and then cooling to 1300 ℃ at the speed of 0.5 ℃/min, and keeping the temperature for 2 hours;
(5) Stopping introducing oxygen, heating to 1560 ℃ at the speed of 0.35 ℃/min, preserving heat for 3 hours, and cooling to obtain the alumina target.
Performance test:
Density testing: the target density was tested using archimedes displacement.
Table 1: performance test meter
Analysis of results:
1. as can be seen from examples 1-3, when the temperature rising rate is increased, the density of the target will be reduced to a certain extent, and we speculate that, probably because the temperature rising rate is increased, closed pores are formed inside the target, the gas cannot be completely removed, so that the density is reduced, but the density is not reduced, and the temperature rising rate is increased, which means that the production time is shortened, so that in practical application, an operator can properly adjust the temperature rising rate according to the density requirement of the product, so as to improve the production efficiency.
2. As can be seen from examples 1 and 4-5, the method for preparing a target according to the present application can realize the manufacture of a multi-sized target, but when the size of the target reaches 1.5mx1m, the density of the target is reduced slightly, and it is presumed that the weight of the target is increased due to the increase of the size, and the friction force of the target placed on alumina sand is increased to affect the shrinkage of the target, so that the density of the target is reduced, but the density of the target still reaches 3.972g/cm 3 despite the reduction of the density of the target.
3. As can be seen from examples 4 and 6, when the pressure during mechanical pressing is increased and the sintering time in step 4 is prolonged, the density of the target is improved to a certain extent, and we speculate that the reason for this phenomenon is that the target blank is denser after the pressure is increased, so that the improvement of the density of the target is promoted; on the other hand, the sintering time in the step 4 is prolonged, so that the target material is more thoroughly contracted, the pores are fewer, and the target material and the pore are synergistic, so that the density of the target material is further improved.
4. As can be seen from examples 1 and 7, when the target was cold isostatic pressed at a pressure of 200MPa, the density thereof was significantly lower than that of 300MPa, and we speculate that, with respect to example 1, lowering the cold isostatic pressing pressure resulted in a decrease in the compaction degree of the alumina powder, and thus in a decrease in the density of the alumina green body, and finally, the result that example 7 was lower in density than example 1 was exhibited.
5. As can be seen from examples 1 and 8, when the temperature is raised to 1300 ℃ in step 4, the raising rate is reduced to facilitate the increase of the target density, and we speculate that the alumina material contracts more at each temperature stage due to the lowering of the raising rate, so that the density is increased.
6. As can be seen from example 1 and comparative example 1, when the temperature is raised to 1550 ℃ at one time in step 4, the target is cracked, and we speculate that the sintering time is too short, which results in incomplete shrinkage, more pores and further reduced target density.
7. As can be seen from example 1 and comparative example 2, when the depressurization time is shortened in step 3, the finally prepared target material is cracked, and it is presumed that, due to the shortened depressurization time, when the pressure is reduced but no pressure maintaining operation is performed, the alumina blank body is relatively expanded when the pressure is lost, thereby causing the cracking of the alumina target material.
8. As can be seen from example 4 and comparative example 1, when an alumina target with a size of 1.5mx1m is produced, the target prepared by the preparation method adopted in comparative example 3 has cracking and density reduction phenomena, and it is supposed that on one hand, the cold isostatic pressure is too high, the pressure release rate is too high, so that the target blank cracks, on the other hand, the sintering time is too short, so that shrinkage is incomplete, and more pores exist, so that the target density is lower.
Claims (5)
1. The preparation method of the alumina target is characterized by comprising the following steps:
Step 1: preparing alumina powder;
Step 2: putting the alumina powder prepared in the step 1 into a die for compression molding to prepare an alumina blank;
Step 3: performing cold isostatic pressing treatment on the alumina blank obtained in the step 2to obtain a high-density alumina blank;
step 4: sintering the high-density alumina blank body obtained in the step 3 at a high temperature to obtain an alumina target material;
the step 4 specifically comprises the following steps: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing the high-density alumina blank body prepared in the step 3 on the alumina sand, heating to 1000 ℃ at a heating rate of 0.5-1 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process;
heating to 1000 deg.C, maintaining for 2-4 hr, heating to 1500-1600 deg.C at a rate of 0.01-0.3 deg.C/min, and maintaining at 30-200 deg.C for 2-10 hr during heating;
Step 4, performing under an air atmosphere;
the density of the alumina target is at least 3.97g/cm 3, and the size of the alumina target is 1500mm multiplied by 1000mm;
The step1 specifically comprises the following steps: adding an alumina raw material into a sand mill, wherein the diameter of a zirconium ball used in the sand milling process is 0.3-0.5mm;
Adding 5% -10% of polyvinyl alcohol solution relative to the content of the alumina raw material into a sand mill while adding the alumina raw material, wherein the content of polyvinyl alcohol in the polyvinyl alcohol solution is 10% -15%, spray drying after finishing sanding, and drying at the inlet temperature of 180-200 ℃ and the outlet temperature of 70-100 ℃ to obtain alumina powder with D90<0.5 mu m;
the step 2 specifically comprises the following steps: loading the alumina powder prepared in the step 1 into a die, setting the pressure to be more than or equal to 16000kN for mechanical pressing, polishing corners of a blank body after mechanical pressing, and then vacuum packaging;
the corner radius R of the corner polishing is 0.5-1mm;
the step 3 specifically comprises the following steps: and (3) carrying out cold isostatic pressing on the packaged alumina blank obtained in the step (2) under the pressure of 200-300 MPa at the pressure increasing rate of 10-20 MPa/min for 5-10min, then reducing the pressure to 0MPa at the pressure reducing rate of 30-50MPa/min, and keeping the pressure and standing for 1min when the pressure is reduced by 50MPa in the pressure reducing process, so as to obtain the alumina blank with high density after the pressure reduction.
2. The method for preparing an alumina target according to claim 1, wherein the step 4 specifically comprises: paving a layer of sintered alumina sand on a sintering bearing plate in a normal pressure sintering furnace, placing the alumina blank body prepared in the step 3 on the alumina sand, heating to 1000 ℃ at a heating rate of 0.6-0.8 ℃/min, and preserving heat for 2-4h at every 200 ℃ in the heating process;
Heating to 1000 ℃ and preserving heat for 2-4h, heating to 1550-1600 ℃ at the speed of 0.05-0.2 ℃/min, and preserving heat for 2-10h at the temperature of 50-100 ℃ in the heating process;
Step 4 is carried out under an air atmosphere.
3. The method of producing an alumina target according to claim 1, wherein the dimensions of the die in step 1 are 1500mm x 1000mm, and the pressure at the time of mechanical pressing is 16000kN to 25000kN.
4. The method for producing an alumina target according to claim 1, wherein in step 2, the alumina powder having a bulk density of 1.0 to 1.2g/cm 3 and a moisture content of 0.8 to 1.2% obtained in step 1 is selected, and is put into a mold and molded.
5. An alumina target prepared by the method of any one of claims 1 to 4.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332929A (en) * | 2013-07-17 | 2013-10-02 | 国家纳米技术与工程研究院 | Forming process of high density large size AZO target material blank body |
| JP2014173133A (en) * | 2013-03-08 | 2014-09-22 | Ube Material Industries Ltd | Target material and production method thereof |
| CN112079626A (en) * | 2020-09-16 | 2020-12-15 | 韶关市欧莱高新材料有限公司 | Aluminum-neodymium-indium-zinc oxide rotary target and preparation method thereof |
| CN112390628A (en) * | 2020-11-23 | 2021-02-23 | 先导薄膜材料（广东）有限公司 | Preparation method of aluminum oxide target material |
| CN112876236A (en) * | 2021-03-04 | 2021-06-01 | 云南戊电靶材科技有限公司 | Preparation method of AZO target material grain size used for thin-film solar cell |
| CN114057481A (en) * | 2020-07-31 | 2022-02-18 | 广州市尤特新材料有限公司 | Method for producing zinc oxide target material and zinc oxide target material |
| CN114436640A (en) * | 2020-11-06 | 2022-05-06 | 湖南七点钟文化科技有限公司 | Preparation method of zinc oxide aluminum alloy target |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102401709B1 (en) * | 2017-02-20 | 2022-05-26 | 스미토모덴키고교가부시키가이샤 | Oxide sintered compact and its manufacturing method, sputtering target, and semiconductor device manufacturing method |
-
2022
- 2022-12-15 CN CN202211615768.0A patent/CN116253560B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014173133A (en) * | 2013-03-08 | 2014-09-22 | Ube Material Industries Ltd | Target material and production method thereof |
| CN103332929A (en) * | 2013-07-17 | 2013-10-02 | 国家纳米技术与工程研究院 | Forming process of high density large size AZO target material blank body |
| CN114057481A (en) * | 2020-07-31 | 2022-02-18 | 广州市尤特新材料有限公司 | Method for producing zinc oxide target material and zinc oxide target material |
| CN112079626A (en) * | 2020-09-16 | 2020-12-15 | 韶关市欧莱高新材料有限公司 | Aluminum-neodymium-indium-zinc oxide rotary target and preparation method thereof |
| CN114436640A (en) * | 2020-11-06 | 2022-05-06 | 湖南七点钟文化科技有限公司 | Preparation method of zinc oxide aluminum alloy target |
| CN112390628A (en) * | 2020-11-23 | 2021-02-23 | 先导薄膜材料（广东）有限公司 | Preparation method of aluminum oxide target material |
| CN112876236A (en) * | 2021-03-04 | 2021-06-01 | 云南戊电靶材科技有限公司 | Preparation method of AZO target material grain size used for thin-film solar cell |
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