CN108249911A - The manufacturing method of magnesia zinc oxide target blankss - Google Patents

The manufacturing method of magnesia zinc oxide target blankss Download PDF

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Publication number
CN108249911A
CN108249911A CN201611245666.9A CN201611245666A CN108249911A CN 108249911 A CN108249911 A CN 108249911A CN 201611245666 A CN201611245666 A CN 201611245666A CN 108249911 A CN108249911 A CN 108249911A
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China
Prior art keywords
magnesia
zinc oxide
powder
target blankss
mixed
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Inventor
姚力军
潘杰
相原俊夫
王学泽
王钜宝
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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Priority to CN201611245666.9A priority Critical patent/CN108249911A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453Shaped 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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention provides a kind of manufacturing method of magnesia zinc oxide target blankss, including:Zinc oxide, magnesia mixed-powder are provided;After the zinc oxide, magnesia mixed-powder are packed into mold, hot-pressing sintering technique is carried out to the zinc oxide, magnesia mixed-powder, forms magnesia oxide zinc-oxide alloy;The magnesia oxide zinc-oxide alloy from the mold is taken out, obtains magnesia zinc oxide target blankss.Compared to normal pressure-sintered or cold pressing forming process scheme, scheme of the present invention can improve the consistency of formed magnesia zinc oxide target blankss and the probability that microhomogeneity, the reduction magnesia zinc oxide target blankss are cracked, allow the magnesia zinc oxide target blankss consistency reach 98% and more than, and make the magnesia zinc oxide target blankss that there is uniform color and luster, so as to improve the performance of formed magnesia zinc oxide target blankss, make the magnesia zinc oxide target blankss that there is stable physical property and meet sputtering target material performance requirement.

Description

The manufacturing method of magnesia zinc oxide target blankss
Technical field
The present invention relates to target as sputter field more particularly to a kind of manufacturing methods of magnesia zinc oxide target blankss.
Background technology
Sputtering technology is one of the conventional process in target as sputter field, with growing, the sputtering target material of sputtering technology Increasingly important role is played in sputtering technology.Sputtering target material is mainly made of target blankss and backboard, wherein, the matter of target blankss Amount has directly influenced the quality of forming film of sputtering target material.
Zinc oxide (ZnO) is a kind of direct band gap broad stopband (3.37eV) group Ⅱ-Ⅵ compound semiconductor material, have compared with Big exciton bind energy (60meV), and zinc oxide or good piezoelectricity, air-sensitive and photoelectric material.Due to zinc oxide structure, Energy band, electrical and optical aspect have many advantages, such as, and there are many production method of zinc-oxide film, therefore zinc oxide should in device There is wide application range with aspect, manufacture transparent electrode, varistor, solar cell window, surface can be used to Acoustic wave device, gas sensor, light emitting diode etc..
At present, magnesia zinc oxide target blankss have been widely used in the high-strength wearables industry such as metal coating, magnetic memory materials Field.In order to ensure the quality of forming film of sputtering target material, not only have to the purity and relative density of magnesia zinc oxide target blankss Very high requirement, while also have very high requirement to the microhomogeneity of magnesia zinc oxide target blankss.
However, the performance that the prior art forms magnesia zinc oxide target blankss is to be improved.
Invention content
The present invention solves the problems, such as to be to provide a kind of manufacturing method of magnesia zinc oxide target blankss, to improve magnesia oxidation The performance of zinc target blankss.
To solve the above problems, the present invention provides a kind of manufacturing method of magnesia zinc oxide target blankss, including:Oxidation is provided Zinc, magnesia mixed-powder;After the zinc oxide, magnesia mixed-powder are packed into mold, the zinc oxide, magnesia are mixed It closes powder and carries out hot-pressing sintering technique, form magnesia oxide zinc-oxide alloy;By the magnesia oxide zinc-oxide alloy from the mold Middle taking-up obtains magnesia zinc oxide target blankss.
Optionally, the step of hot-pressing sintering technique includes:By the mould equipped with the zinc oxide, magnesia mixed-powder Tool is placed in hot pressing furnace;The hot pressing furnace is carried out to be evacuated to predetermined vacuum value;The hot pressing furnace reaches the predetermined vacuum After value, hot pressed sintering is carried out to the zinc oxide, magnesia mixed-powder.
Optionally, the predetermined vacuum value is less than 100Pa.
Optionally, the step of carrying out hot pressed sintering to the zinc oxide, magnesia mixed-powder includes:With the first heating speed Rate carries out the first heating operation to the hot pressing furnace, the hot pressing furnace is made to be warming up to the first preset temperature, and at described first liter In warm operating process, it is first pressure value to keep the pressure that the mold is subject to;It is default that the hot pressing furnace is warming up to described first After temperature, the second warming temperature is carried out to the hot pressing furnace with the second heating rate, the hot pressing furnace is made to be warming up to second default Temperature;After the hot pressing furnace is warming up to second preset temperature, heat preservation operation is carried out to the mold;The heat preservation operation knot Shu Hou carries out boost operations, until the compressive load per unit area that the mold is subject to reaches with default rate of pressure rise to the mold Second pressure value;Under second preset temperature and second pressure value, heat-insulation pressure keeping operation is carried out to the mold.
Optionally, the first heating rate be 5 degrees celsius/minutes to 10 degrees celsius/minutes, first preset temperature It is 900 degrees Celsius to 1000 degrees Celsius.
Optionally, the first pressure value is 10 tons to 15 tons.
Optionally, second heating rate be 3 degrees celsius/minutes to 5 degrees celsius/minutes, second preset temperature It is 1200 degrees Celsius to 1500 degrees Celsius.
Optionally, in the step of heat preservation operation is carried out to the mold, soaking time is 1 hour to 2 hours.
Optionally, the default rate of pressure rise be 1 tons minute to 5 tons minutes, the second pressure value for 20MPa extremely 30MPa。
Optionally, in the step of carrying out heat-insulation pressure keeping operation to the mold, the time of heat-insulation pressure keeping is 30 minutes to 60 Minute.
Optionally, the step of providing the zinc oxide, magnesia mixed-powder includes:Zinc oxide powder and magnesia are provided Powder;Mechanical mixture is carried out to the Zinc oxide powder and magnesium oxide powder using mixed powder machine, forms zinc oxide, magnesia mixing Powder.
Optionally, the mass ratio of the Zinc oxide powder and magnesium oxide powder is 77:23 to 97:3.
Optionally, the technique of the mechanical mixture is wet blending process;Using mixed powder machine to the Zinc oxide powder and oxidation Magnesium dust was carried out in the step of mechanical mixture, and solvent, the Zinc oxide powder and magnesium oxide powder are added in into the mixed powder machine Mixed slurry is formed after mixing;After the mechanical mixture, the manufacturing method further includes:The mixed slurry is placed in drying Processing is dried in case, and screening granulation processing is carried out after drying process.
Optionally, the solvent is industrial alcohol, pure water or carbon tetrachloride solution.
Optionally, in the step of carrying out mechanical mixture to the Zinc oxide powder and magnesium oxide powder using mixed powder machine, to Medium ball is added in the mixed powder machine.
Optionally, the medium ball and the zinc oxide, the mass ratio of magnesia mixed-powder are 1:1 to 1:3.
Optionally, the medium ball includes two kinds in the first zirconia ball, the second zirconia ball and third zirconia ball Or three kinds, and the diameter of first zirconia ball, the second zirconia ball and third zirconia ball is different.
Optionally, a diameter of 10 millimeters of first zirconia ball, a diameter of 20 millimeters of second zirconia ball, A diameter of 30 millimeters of the third zirconia ball.
Optionally, the medium ball include the first zirconia ball, the second zirconia ball and third zirconia ball, described first The mass ratio of zirconia ball, the second zirconia ball and third zirconia ball is 1:1:1 to 1:2:3.
Optionally, after forming the magnesia oxide zinc-oxide alloy, by the magnesia oxide zinc-oxide alloy from the mold Before taking-up, the manufacturing method further includes:Pressure cooling is carried out to the mold.
Optionally, after the magnesia oxide zinc-oxide alloy is taken out from the mold, the magnesia zinc oxide is obtained The step of target blankss, further includes:Wire cutting technology is carried out to the magnesia oxide zinc-oxide alloy, forms magnesia zinc oxide primary target Base;Grinding is carried out to the initial target blankss of the magnesia zinc oxide, forms the magnesia zinc oxide target blankss.
Compared with prior art, technical scheme of the present invention has the following advantages:
After the zinc oxide provided, magnesia mixed-powder are packed into mold by the present invention, the zinc oxide, magnesia are mixed Powder carries out hot-pressing sintering technique, forms magnesia oxide zinc-oxide alloy;By the magnesia oxide zinc-oxide alloy from the mold After taking-up, magnesia zinc oxide target blankss are obtained.Compared to normal pressure-sintered or cold pressing forming process scheme, scheme of the present invention can To improve the consistency of institute's formation magnesia zinc oxide target blankss and microhomogeneity, the reduction magnesia zinc oxide target The cracked probability of base, allow the magnesia zinc oxide target blankss consistency reach 98% and more than, and make the oxygen Changing magnesium zinc oxide target blankss has uniform color and luster, so as to improve the performance of formed magnesia zinc oxide target blankss, makes the oxidation Magnesium zinc oxide target blankss have stable physical property and meet sputtering target material performance requirement.
In alternative, the step of providing the zinc oxide, magnesia mixed-powder, includes:Zinc oxide powder and oxygen are provided Change magnesium dust;Mechanical mixture is carried out to the Zinc oxide powder and magnesium oxide powder using mixed powder machine, forms zinc oxide, magnesia Mixed-powder;The present invention carries out mechanical mixture using mixed powder machine to Zinc oxide powder and magnesium oxide powder, makes the oxide powder and zinc End and magnesium oxide powder can be mixed more uniformly, prepare ingredient uniformly and zinc oxide, the magnesia of segregation-free mix Powder is closed, efficiently solves zinc oxide, magnesia mixed-powder draws due to the density difference of Zinc oxide powder and magnesium oxide powder The segregation lamination risen, so as to improve the microhomogeneity of formed magnesia zinc oxide target blankss.
In alternative, the technique of the mechanical mixture is wet blending process, and the wet blending process can reduce the oxidation The probability that zinc, magnesia mixed-powder lump is conducive to improve mixed powder uniformity, and oxidation is formed so as to be conducive to improve The microhomogeneity of magnesium zinc oxide target blankss.
In alternative, in the step of zinc oxide, magnesia mixed-powder progress hot pressed sintering, elder generation is Celsius with 5 Degree/min the hot pressing furnace is made to be warming up to 900 degrees Celsius to 1000 degrees Celsius to the heating rates of 10 degrees celsius/minutes;It is described After hot pressing furnace reaches 900 degrees Celsius to 1000 degrees Celsius, institute is made with the heating rate of 3 degrees celsius/minutes to 5 degrees celsius/minutes It states hot pressing furnace and is warming up to 1200 degrees Celsius to 1500 degrees Celsius, and heat preservation 1 is carried out reaching 1200 degrees Celsius to 1500 degrees Celsius Hour was to 2 hours;After heat preservation, boost operations are carried out to the mold with the rate of pressure rise of 1 tons minute to 5 tons minutes, Until the compressive load per unit area that the mold is subject to reaches 20MPa to 30MPa, and keep the temperature and protect under the conditions of the temperature and pressure Pressure 30 minutes to 60 minutes.The present invention is forming the magnesia oxidation by setting rational processing step and technological parameter During zinc target blankss, make each zone oxidation zinc, magnesia mixed-powder in the mold that can be pressurized with thermally equivalent, so as to have The consistency and microhomogeneity of magnesia zinc oxide target blankss are formed conducive to raising.
Description of the drawings
Fig. 1 is the flow diagram of one embodiment of manufacturing method of magnesia zinc oxide target blankss of the present invention;
Fig. 2 is the flow diagram corresponding to step S1 in embodiment illustrated in fig. 1;
Fig. 3 is the structure diagram corresponding to step S1 in embodiment illustrated in fig. 1;
Fig. 4 is the flow diagram corresponding to step S2 in embodiment illustrated in fig. 1;
Fig. 5 is the structure diagram corresponding to step S2 in embodiment illustrated in fig. 1;
Fig. 6 is the flow diagram corresponding to step S23 in Fig. 4;
Fig. 7 is the structure diagram corresponding to step S3 in embodiment illustrated in fig. 1.
Specific embodiment
By background technology it is found that the prior art performance that forms magnesia zinc oxide target blankss is to be improved.Analyze its original Because being:
The manufacturing process of magnesia zinc oxide target blankss be mainly it is normal pressure-sintered or mixing after cold moudling.Therefore oxygen is formed The consistency for changing magnesium zinc oxide target blankss is relatively low, and processing performance, microhomogeneity and surface uniformity are poor, and easily go out The problem of existing crackle, being difficult to reach the industries such as semiconductor, solar energy, LCD so as to cause formed magnesia zinc oxide target blankss makes With requiring.Therefore be badly in need of providing a kind of sintering process of magnesia zinc oxide target blankss, with ensure formation magnesia zinc oxide target Base can meet the performance requirement of sputtering target material.
To solve the above-mentioned problems, the present invention provides a kind of manufacturing method of magnesia zinc oxide target blankss, including:Oxygen is provided Change zinc, magnesia mixed-powder;After the zinc oxide, magnesia mixed-powder are packed into mold, to the zinc oxide, magnesia Mixed-powder carries out hot-pressing sintering technique, forms magnesia oxide zinc-oxide alloy;By the magnesia oxide zinc-oxide alloy from the mould It is taken out in tool, obtains magnesia zinc oxide target blankss.
After the zinc oxide provided, magnesia mixed-powder are packed into mold by the present invention, the zinc oxide, magnesia are mixed Powder carries out hot-pressing sintering technique, forms magnesia oxide zinc-oxide alloy;By the magnesia oxide zinc-oxide alloy from the mold After taking-up, magnesia zinc oxide target blankss are obtained.Compared to normal pressure-sintered or cold pressing forming process scheme, scheme of the present invention can To improve the consistency of institute's formation magnesia zinc oxide target blankss and microhomogeneity, the reduction magnesia zinc oxide target The cracked probability of base, allow the magnesia zinc oxide target blankss consistency reach 98% and more than, and make the oxygen Changing magnesium zinc oxide target blankss has uniform color and luster, so as to improve the performance of formed magnesia zinc oxide target blankss, makes the oxidation Magnesium zinc oxide target blankss have stable physical property and meet sputtering target material performance requirement.
It is understandable for the above objects, features and advantages of the present invention is enable to become apparent, below in conjunction with the accompanying drawings to the present invention Specific embodiment be described in detail.
It please referring to Fig.1, Fig. 1 is the flow diagram of one embodiment of manufacturing method of magnesia zinc oxide target blankss of the present invention, The manufacturing method of the present embodiment magnesia zinc oxide target blankss includes following basic step:
Step S1:Zinc oxide, magnesia mixed-powder are provided;
Step S2:After the zinc oxide, magnesia mixed-powder are packed into mold, the zinc oxide, magnesia are mixed Powder carries out hot-pressing sintering technique, forms magnesia oxide zinc-oxide alloy;
Step S3:The magnesia oxide zinc-oxide alloy from the mold is taken out, obtains magnesia zinc oxide target blankss.
In order to which the production method of the magnesia zinc oxide target blankss of the embodiment of the present invention is better described, below in conjunction with reference Fig. 2 to Fig. 7, is further described specific embodiments of the present invention.
With reference to referring to figs. 1 to Fig. 3, Fig. 2 shows the flow diagram corresponding to step S1 in embodiment illustrated in fig. 1, Fig. 3 Show the structure diagram corresponding to step S1 in embodiment illustrated in fig. 1.Step S1 is performed, provides zinc oxide, magnesia mixes Close powder 103 (as shown in Figure 3).
The zinc oxide, magnesia mixed-powder 103 provide Process ba- sis to be subsequently formed magnesia oxide zinc-oxide alloy.
Specifically, with reference to referring to figs. 2 and 3, step S11 is performed, Zinc oxide powder 101 (as shown in Figure 3) and oxygen are provided Change magnesium dust 102 (as shown in Figure 3).
In the present embodiment, the Zinc oxide powder 101 and magnesium oxide powder 102 are high-purity powder of more than 99.9% purity End, so as to allow subsequently formed magnesia zinc oxide target blankss purity reach 99.9% and more than.And according to actual process The mass ratio of demand, the Zinc oxide powder 101 and magnesium oxide powder 102 is 77:23 to 97:3.
In the present embodiment, the granularity of the Zinc oxide powder 101 is 2 microns to 3 microns, the magnesium oxide powder 102 Granularity is 2 microns to 3 microns.By the selected Zinc oxide powder 101 of reasonable particle size and magnesium oxide powder 102, with control The follow-up crystallite dimension for forming magnesia oxide zinc-oxide alloy, while the grain of the Zinc oxide powder 101 and magnesium oxide powder 102 Degree is smaller, also helps the progress of follow-up hot-pressing sintering technique.
With reference to referring to figs. 2 and 3, step S12 is performed, using mixed powder machine to the Zinc oxide powder 101 and magnesia powder End 102 carries out mechanical mixture, forms zinc oxide, magnesia mixed-powder 103 (as shown in Figure 3).
By carrying out mechanical mixture to the Zinc oxide powder 101 and magnesium oxide powder 102, make the Zinc oxide powder 101 and magnesium oxide powder 102 can be uniformly mixed together, prepare ingredient uniformly and segregation-free zinc oxide, magnesia Mixed-powder 103 efficiently solves formed zinc oxide, magnesia mixed-powder 103 because of the Zinc oxide powder 101 and oxidation Lamination is segregated caused by the density difference of magnesium dust 102, to be subsequently formed the magnesia oxide zinc-oxide alloy of better quality Process ba- sis is provided.
Wherein, in the step of carrying out mechanical mixture to the Zinc oxide powder 101 and magnesium oxide powder 102, according to follow-up The mass percentage content of zinc oxide and magnesia in formed magnesia zinc oxide target blankss, by 101 He of Zinc oxide powder The mass ratio setting of magnesium oxide powder 102 is in the reasonable scope.
In the present embodiment, by the Zinc oxide powder 101 and magnesium oxide powder 102 according to mass ratio 77:23 to 97:3 Ratio mixes powder machine with ball milling and carries out mechanical mixture.Wherein, 102 respective quality of the Zinc oxide powder 101 and magnesium oxide powder Depending on the actual size demand of follow-up formed magnesia oxide zinc-oxide alloy.
It should be noted that the incorporation time of the mechanical mixture technique is unsuitable too short, it is also unsuitable long.If the machine The incorporation time of tool mixing is too short, since the mixing of the Zinc oxide powder 101 and magnesium oxide powder 102 is uniform not enough, holds Formed zinc oxide, the appearance segregation lamination of magnesia mixed-powder 103 are easily led to, subsequently magnesia is formed so as to reduce The physical property and processing performance of oxide zinc-oxide alloy;If the incorporation time of the mechanical mixture is long, in the oxide powder and zinc End 101 and magnesium oxide powder 102 easily cause the problem of temperature is excessively high during mixing, so as to be easy to cause the zinc oxide Powder 101 and magnesium oxide powder 102 aoxidize.For this purpose, in the present embodiment, the incorporation time of the mechanical mixture is 10 hours To 30 hours.
In the present embodiment, the technique of the mechanical mixture is wet blending process.Correspondingly, using mixed powder machine to the zinc oxide In the step of powder 101 and magnesium oxide powder 102 carry out mechanical mixture, mixed to the ball milling and solvent is added in powder machine, the oxygen Mixed slurry is formed after changing zinc powder 101 and the mixing of magnesium oxide powder 102.
The Zinc oxide powder 101 and magnesium oxide powder 102 form mixed slurry, therefore the wet blending process can after mixing To reduce the probability that lumps of institute formation zinc oxide, magnesia mixed-powder 103, be conducive to improve mixed powder uniformity, thus Be conducive to improve the follow-up microhomogeneity for forming magnesia oxide zinc-oxide alloy.
In the present embodiment, the solvent is industrial alcohol of the concentration more than 99.99%.The industrial alcohol has preferable Effumability, consequently facilitating subsequently being dried to form dry zinc oxide, magnesia mixed powder to the mixed slurry End 103.In other embodiments, the solvent can also be pure water or carbon tetrachloride solution.
It should be noted that in order to preferably be uniformly mixed the Zinc oxide powder 101 and magnesium oxide powder 102, adopt It is mixed in the step of powder machine carries out mechanical mixture to the Zinc oxide powder 101 and magnesium oxide powder 102 with the ball milling, to described Ball milling mixes in powder machine addition medium ball (not shown), mix powder it is uniform after, then the medium ball taken out.
In the present embodiment, the material of the medium ball is zirconium oxide.Zirconia material is wear-resistant material, in mechanical mixture mistake The phenomenon that material is fallen is not susceptible in journey, and is not easy to react with the Zinc oxide powder 101 or magnesium oxide powder 102, So as to prevent the introducing of impurity element.
It should be noted that in order to avoid being generated to the mixed powder effect of the Zinc oxide powder 101 and magnesium oxide powder 102 Harmful effect, the medium ball and the zinc oxide, magnesia mixed-powder 103 mass ratio be 1:1 to 1:3.
Specifically, the medium ball includes two kinds in the first zirconia ball, the second zirconia ball and third zirconia ball Or three kinds, and the diameter of first zirconia ball, the second zirconia ball and third zirconia ball is different.Different-diameter Medium ball can increase the area of phase mutual friction and shearing between the medium ball, so as to improve ball milling effect, and then improve institute State the mixed powder uniformity of Zinc oxide powder 101 and magnesium oxide powder 102.
In the present embodiment, a diameter of 10 millimeters of first zirconia ball, a diameter of the 20 of second zirconia ball Millimeter, a diameter of 30 millimeters of the third zirconia ball.
In the present embodiment, the medium ball includes the first zirconia ball, the second zirconia ball and third zirconia ball, and institute The mass ratio for stating the first zirconia ball, the second zirconia ball and third zirconia ball is 1:1:1 to 1:2:3.By rationally controlling The mass ratio of three kinds of zirconia balls, it is uniform so as to be conducive to improve the mixed powder of the Zinc oxide powder 101 and magnesium oxide powder 102 Property.
In the present embodiment, the Zinc oxide powder 101 and magnesium oxide powder 102 form mixed slurry after mechanical mixture, Therefore after the mechanical mixture, the manufacturing method further includes:The mixed slurry is placed in drying box, place is dried Reason, and screening granulation processing is carried out after drying process.
In the present embodiment, the temperature of the drying process is 110 DEG C to 130 DEG C;And while in order to ensure drying effect, The waste of process time and cost is avoided, the time of the drying process is 1 hour to 5 hours.
In the present embodiment, in order to improve the caking of the Zinc oxide powder 101 and magnesium oxide powder 102 after mechanical mixture Phenomenon after the drying process, uses size of mesh to carry out screening granulation processing for 1 millimeter of sieve, with broken caking, shape Into the mixed-powder of better quality.
With reference to reference to figure 1, Fig. 4, Fig. 5 and Fig. 6, step S2 is performed, by the zinc oxide, magnesia mixed-powder 103 (such as Shown in Fig. 3) be packed into mold 150 (as shown in Figure 5) after, to the zinc oxide, the progress hot pressed sintering work of magnesia mixed-powder 103 Skill forms magnesia oxide zinc-oxide alloy 300 (as shown in Figure 5).
The magnesia oxide zinc-oxide alloy 300 provides Process ba- sis to be subsequently formed magnesia zinc oxide target blankss.
Flow diagram with reference to corresponding to showing step S2 in embodiment illustrated in fig. 1 with reference to figure 4 and Fig. 5, Fig. 4, Fig. 5 Show the structure diagram corresponding to step S2 in embodiment illustrated in fig. 1.In the present embodiment, the step of the hot-pressing sintering technique Suddenly include:Step S21 is performed, the mold 150 equipped with the zinc oxide, magnesia mixed-powder 103 is placed in hot pressing furnace 100 In (as shown in Figure 5);Step S22 is performed, the hot pressing furnace 100 is carried out being evacuated to predetermined vacuum value;Step S23 is performed, After the hot pressing furnace 100 reaches the predetermined vacuum value, hot pressed sintering is carried out to the zinc oxide, magnesia mixed-powder 103.
Specifically, step S21 is performed, the mold 150 equipped with the zinc oxide, magnesia mixed-powder 103 is placed in heat It presses in stove 100.
After forming the zinc oxide, magnesia mixed-powder 103, the zinc oxide, magnesia mixed-powder 103 are placed in In mold 150, the mold 150 is used to limit the follow-up shape for forming magnesia oxide zinc-oxide alloy 300, is additionally operable to protection institute State zinc oxide, magnesia mixed-powder 103.
The mold 150 is placed in the process environments of follow-up hot pressed sintering, therefore the mold 150 has preferable heat conduction Property and heat-resisting quantity, and with higher mechanical strength, during so as to avoid follow-up hot pressed sintering the mold 150 deform upon or Cracking, and can ensure that the mold 150 is not sent out during hot pressed sintering with the zinc oxide, magnesia mixed-powder 103 Raw reaction.For this purpose, in the present embodiment, the material of the mold 150 is graphite.
The hot pressing furnace 100 provides technique subsequently to carry out hot pressed sintering to the zinc oxide, magnesia mixed-powder 103 Place.
In the present embodiment, the mold 150 further includes seaming chuck 110 (as shown in Figure 5) and push-down head 120 (such as Fig. 5 institutes Show), after the zinc oxide, magnesia mixed-powder 103 are packed into the mold 150, the zinc oxide, magnesia mixed powder End 103 is between the seaming chuck 110 and push-down head 120;Wherein, the push-down head 120 is used to carry the zinc oxide, oxygen Change magnesium mixed-powder 103, can also be used to touch with to the mold with 150 bottom connection of mold according to actual process demand 150 apply pressure;When the mold 150 is placed in hot pressing furnace 100, the seaming chuck 110 is located at 150 over top of mold And be not in contact with 150 top of mold, subsequently under the conditions of heating process, the seaming chuck 110 is pushed up with the mold 150 Portion is in contact to apply pressure to the mold 150, to realize that the hot pressing to the zinc oxide, magnesia mixed-powder 103 is burnt Knot, so as to form magnesia oxide zinc-oxide alloy 300.
It should be noted that the mold 150 is hollow barrel structure, therefore in the present embodiment, 110 He of seaming chuck Between the zinc oxide, magnesia mixed-powder 103 and the push-down head 120 and the zinc oxide, magnesia mixed-powder Gasket 155 is further respectively had between 103, between the seaming chuck 110 and the zinc oxide, magnesia mixed-powder 103 Gasket 155 for top as the mold 150, positioned at the push-down head 120 and the zinc oxide, magnesia mixed powder Gasket 155 between end 103 is for the bottom as the mold 150.
The gasket 155 can play buffer action, and institute is in direct contact to avoid the seaming chuck 110 and push-down head 120 State zinc oxide, magnesia mixed-powder 103;Therefore in subsequent technique, by applying stressed mode to the gasket 155, To realize the hot pressed sintering of the zinc oxide, magnesia mixed-powder 103.In the present embodiment, the material of the gasket 155 is stone Ink.The aforementioned selected analysis to 150 material of mold can refer to the selected analysis of 155 material of gasket, details are not described herein.
In addition, in order to cost-effective, it can be simultaneously to more parts of zinc oxide, magnesia mixed powder in every heat hot-pressing sintering technique End 103 carries out hot pressed sintering;In order to which the more parts of zinc oxide, magnesia mixed-powder 103 are isolated, each part zinc oxide, The gasket 155 is additionally provided between magnesia mixed-powder 103.Wherein, according to follow-up formed magnesia oxide zinc-oxide alloy 300 150 total height of thickness and the mold difference, per heat hot pressed sintering in zinc oxide, magnesia mixed-powder 103 Number is also different, correspondingly, the quantity of the gasket 155 is also different.
It should also be noted that, in order to improve the surface smoothness of the zinc oxide, magnesia mixed-powder 103, to carry It is high subsequently form the quality of magnesia oxide zinc-oxide alloy 300 and make the mold 150 accommodate more the zinc oxide, Magnesia mixed-powder 103, to achieve the purpose that the mold more than 150 fills product, by the zinc oxide, magnesia mixed-powder After 103 are placed in the mold 150, the manufacturing method further includes:Using static pressure machine to the zinc oxide, magnesia mixed powder End 103 applies the pressure of 5MPa, to realize that the pre-molding of the zinc oxide, magnesia mixed-powder 103 is handled, by the oxygen Change zinc, magnesia mixed-powder 103 is compacted.
Step S22 is performed, the hot pressing furnace 100 (as shown in Figure 5) is carried out being evacuated to predetermined vacuum value.
By being vacuumized to the hot pressing furnace 100, to ensure that there is certain vacuum degree in the hot pressing furnace 100, it is The follow-up hot pressed sintering that carries out provides Process ba- sis.
In the present embodiment, in the step of being vacuumized to the hot pressing furnace 100, the predetermined vacuum value is less than 100Pa.
Step S23 is performed, after the hot pressing furnace 100 (as shown in Figure 5) reaches the predetermined vacuum value, to the oxidation Zinc, magnesia mixed-powder 103 are (as shown in Figure 3) to carry out hot pressed sintering.
By carrying out hot pressed sintering to the zinc oxide, magnesia mixed-powder 103, to form magnesia oxide zinc-oxide alloy 300 (as shown in Figure 5).
Below in conjunction with Fig. 5 and Fig. 6, Fig. 6 is the flow diagram corresponding to step S23 in Fig. 4, in the present invention to described The step of zinc oxide, magnesia mixed-powder 103 carry out hot pressed sintering illustrates.
Specifically, step S231 is performed, the first heating operation is carried out to the hot pressing furnace 100 with the first heating rate, is made The hot pressing furnace 100 is warming up to the first preset temperature, and in the first heating operating process, keep the mold 150 by The pressure arrived is first pressure value.
It is operated by the first heating, makes the lattice of each material and crystalline substance in the zinc oxide, magnesia mixed-powder 103 Plastic Flow is concurrently given birth in boundary's phase counterdiffusion, so as to fulfill the zinc oxide, the first one-step forming of magnesia mixed-powder 103, after being Continuous second warming temperature that carries out provides good Process ba- sis.
It should be noted that in the present embodiment, before the first heating operation is not carried out, the seaming chuck 110 It is in contact in 150 over top of mold and not with 150 top of mold, correspondingly, not carrying out the first heating Before operation, the pressure size that the mold 150 is subject to is zero.
But during the first heating operation is carried out, the zinc oxide, magnesia mixed-powder 103 occur Thermal expansion, correspondingly, gasket 155 between the seaming chuck 110 and the zinc oxide, magnesia mixed-powder 103 is along direction The direction of the seaming chuck 110 is moved, so as to which the seaming chuck 110 be made to be in contact with the gasket 155;And with temperature Be continuously increased, the zinc oxide, magnesia mixed-powder 103 degree of thermal expansion accordingly increase, so as to passing through the gasket 155 contacts with the seaming chuck 110 and extruding make the gasket 155 be pressurized, and the pressure that the gasket 155 is subject to acts on On the zinc oxide, magnesia mixed-powder 103.
Therefore, in order to avoid the zinc oxide, magnesia mixed-powder 103 be pressurized it is excessive, when the zinc oxide, magnesia When the pressure that the gasket 155 is subject to when mixed-powder 103 expands is more than first pressure value, by making 110 edge of seaming chuck The mode of direction movement far from 150 top of mold, to reduce the pressure that the gasket 155 is subject to, makes the mold 150 The pressure being subject to is maintained at first pressure value, until the hot pressing furnace 100 is warming up to the first preset temperature.
In the present embodiment, while the zinc oxide, magnesia mixed-powder 103 is avoided to be pressurized excessive, described in guarantee The preliminary molding effect of zinc oxide, magnesia mixed-powder 103, the first pressure value are 10 tons to 15 tons.Wherein, 1 ton of phase When in 1000 kilograms, that is, the pressure of 9800 newton.
In the present embodiment, with the first heating rate to the hot pressing furnace 100 carry out the first heating operation the step of in, it is described First preset temperature is unsuitable too low, also unsuitable excessively high.If first preset temperature is too low, the zinc oxide, magnesia Mixed-powder 103 easily causes preliminary molding effect poor due to heated deficiency, is unfavorable for subsequently forming magnesia zinc oxide The consistency and microhomogeneity of alloy 300;If first preset temperature is excessively high, the zinc oxide, magnesia mix It is excessively high to close the energy that each material obtains in powder 103, the excessive velocities buried in oblivion mutually are merged, so as to be difficult to realize the mold The effect that each zone oxidation zinc, magnesia mixed-powder 103 are heated evenly in 150.For this purpose, in the present embodiment, described first is pre- If temperature is 900 degrees Celsius to 1000 degrees Celsius.
The first heating rate is unsuitable too small, also should not be too large.If the first heating rate is too small, accordingly reach Process time needed for first preset temperature increases, so as to cause the decline of manufacture efficiency;If the first heating speed Rate is excessive, then is easily reduced the being heated evenly property of each zone oxidation zinc, magnesia mixed-powder 103 in the mold 150, unfavorable In the follow-up microhomogeneity for forming magnesia oxide zinc-oxide alloy 300.For this purpose, in the present embodiment, the first heating Rate is 5 degrees celsius/minutes to 10 degrees celsius/minutes.
Step S232 is performed, after the hot pressing furnace 100 is warming up to first preset temperature, with the second heating rate to institute It states hot pressing furnace 100 and carries out the second warming temperature, the hot pressing furnace 100 is made to be warming up to the second preset temperature.
By second warming temperature, further promote each material in the zinc oxide, magnesia mixed-powder 103 Simultaneously Plastic Flow occurs for lattice and Grain-Boundary Phase counterdiffusion, and provides Process ba- sis for subsequent heat preservation operation.
Second preset temperature is unsuitable too low, also unsuitable excessively high.When second preset temperature is too low, then it is easy to cause The zinc oxide, 103 each material of magnesia mixed-powder are difficult to obtain enough diffusion activation energies, so as to cause the oxidation Zinc, the hot pressed sintering effect of magnesia mixed-powder 103 are poor, and then cause subsequently to form magnesia oxide zinc-oxide alloy 300 Consistency decline;When first preset temperature is excessively high, excessively high technological temperature makes the mold 150 be in rugged environment In, it can accordingly increase process risk.For this purpose, in the present embodiment, second preset temperature is Celsius for 1200 degrees Celsius to 1500 Degree.
Second heating rate is unsuitable too low, also unsuitable excessively high.When second heating rate is too small, accordingly reach institute Stating the process time needed for the second preset temperature increases, so as to cause the decline of manufacture efficiency;When the second heating rate mistake When big, being then the heated evenly property of each zone oxidation zinc, magnesia mixed-powder 103 in the mold 150 is easily reduced, is unfavorable for The follow-up microhomogeneity for forming magnesia oxide zinc-oxide alloy 300.For this purpose, in the present embodiment, the second heating speed Rate is 3 degrees celsius/minutes to 5 degrees celsius/minutes.
Step S233 is performed, after the hot pressing furnace 100 is warming up to second preset temperature, the mold 150 is carried out Heat preservation operation.
During the heat preservation operation, to reaching subregion zinc oxide, the magnesia of second preset temperature Mixed-powder 103 is kept the temperature, to being not up to subregion zinc oxide, the magnesia mixed-powder of second preset temperature 103 continue to heat up, that is to say, that and spread even heat by the heat preservation operation, it is described after the heat preservation operation is completed Each zone oxidation zinc in mold 150, magnesia mixed-powder 103 temperature can reach second preset temperature;Therefore The heat preservation operation is subsequently carries out the zinc oxide, magnesia mixed-powder 103 boost operations and heat-insulation pressure keeping operation Good Process ba- sis is provided, so as to improve the hot pressed sintering effect of the zinc oxide, magnesia mixed-powder 103, into And improve the consistency and microhomogeneity for subsequently forming magnesia oxide zinc-oxide alloy 300.
It should be noted that in the step of carrying out heat preservation operation to the mold 150, soaking time is unsuitable too short, also not It is preferably long.If the soaking time is too short, it is difficult to improve the zinc oxide, 103 hot pressed sintering of magnesia mixed-powder effect The uniformity of fruit can accordingly reduce the follow-up consistency and microhomogeneity for forming magnesia oxide zinc-oxide alloy 300;Such as Soaking time is long described in fruit, when being difficult to further improve consistency and microhomogeneity, waste of energy, reduction instead Manufacture efficiency or even generation process risk.For this purpose, in the present embodiment, the soaking time is 1 hour to 2 hours.
Step S234 is performed, after the heat preservation operation, boosting behaviour is carried out to the mold 150 with default rate of pressure rise Make, until the compressive load per unit area that the mold 150 is subject to reaches second pressure value.
Pressure (direction of exerting pressure is as shown in arrow 105 in Fig. 5) is applied to the mold 150 by the boost operations, is made Each material obtains diffusion activation energy in the zinc oxide, magnesia mixed-powder 103, so as to for subsequently to the zinc oxide, oxygen Change magnesium mixed-powder 103 and heat-insulation pressure keeping operation offer Process ba- sis is provided.
The second pressure value is unsuitable too small, also should not be too large.If the second pressure value is too small, due to the mold 150 compressive loads per unit area being subject to are not big enough, and the zinc oxide, 103 each material of magnesia mixed-powder is caused to be difficult to obtain foot Enough diffusion activation energies, the hot pressed sintering effect so as to cause the zinc oxide, magnesia mixed-powder 103 is poor, and then leads It causes subsequently to form the consistency of magnesia oxide zinc-oxide alloy 300 and microhomogeneity decline;If the second pressure It is worth excessive, waste of energy or even when the compressive load per unit area that the mold 150 is subject to is excessive, makes at the mold 150 instead In rugged environment, it can accordingly increase process risk.For this purpose, in the present embodiment, the second pressure value for 20MPa extremely 30MPa, i.e., the value of compressive load per unit area that described gasket 155 is subject to are 20MPa to 30MPa, that is to say, that the zinc oxide, The value for the compressive load per unit area that magnesia mixed-powder 103 is subject to is 20MPa to 30MPa.
Default rate of pressure rise is unsuitable too small, also should not be too large.If rate of pressure rise is too small, accordingly reach the second pressure Process time needed for value increases, so as to cause the decline of manufacture efficiency;If rate of pressure rise is excessive, it is easily reduced the mould The compression uniformity of each zone oxidation zinc, magnesia mixed-powder 103 in tool 150 is unfavorable for subsequently forming magnesia oxidation The microhomogeneity of kirsite 300.For this purpose, in the present embodiment, the default rate of pressure rise is 1 tons minute to 5 tons/point Clock.Wherein, 1000 kilograms, that is, the pressure of 9800 newton are equivalent to for 1 ton.
Step S235 is performed, under second preset temperature and second pressure value, heat preservation guarantor is carried out to the mold 150 Press operation.
In the present embodiment, after the heat-insulation pressure keeping operation, magnesia oxide zinc-oxide alloy 300 is formed.
It is operated by the heat-insulation pressure keeping, under second preset temperature, the unit area that is subject to the mold 150 Pressure value can reach second pressure value, so as to improve each zone oxidation zinc, magnesia mixed-powder in the mold 150 103 compression uniformity;Accordingly improve the zinc oxide, magnesia mixed-powder 103 hot pressed sintering effect uniformity, into And the consistency and microhomogeneity of the magnesia oxide zinc-oxide alloy 300 can be improved.
It should be noted that in the step of carrying out heat-insulation pressure keeping operation to the mold 150, the time of heat-insulation pressure keeping is unsuitable It is too short, it is also unsuitable long.If the heat-insulation pressure keeping time is too short, each zone oxidation zinc in the mold 150, oxidation are improved The effect unobvious of the compression uniformity of magnesium mixed-powder 103;If the overlong time of the heat-insulation pressure keeping, for formed oxygen When the consistency and microhomogeneity of change magnesium oxide zinc-oxide alloy 300 are had reached preferably, waste of energy, reduction manufacture instead Efficiency or even easily generate process risk.For this purpose, in the present embodiment, the time of heat-insulation pressure keeping is 30 minutes to 60 minutes.
With continued reference to Fig. 4, it should be noted that after forming the magnesia oxide zinc-oxide alloy 300 (as shown in Figure 5), institute Manufacturing method is stated to further include:Step S24 is performed, pressure cooling is carried out to the mold 150 (as shown in Figure 5).
In the present embodiment, after completing the hot-pressing sintering technique, the hot pressing furnace 100 (as shown in Figure 5) is closed, is then adopted The mold 150 is made to go to press and cool down naturally with the method for furnace cooling.When the temperature in the hot pressing furnace 100 is less than 200 DEG C When, at for example, 25 DEG C to 200 DEG C, by the mold 150 equipped with the magnesia oxide zinc-oxide alloy 300 from the hot pressing furnace 100 Interior taking-up.
Specifically, by being passed through inert gas into the hot pressing furnace 100, make to reach negative pressure in the hot pressing furnace 100, from And air is promoted to enter in the hot pressing furnace 100, and then realize that the mold 150 goes the effect of pressure naturally.In the present embodiment, institute Inert gas is stated as argon gas, after being passed through inert gas into the hot pressing furnace 100, the pressure that makes the hot pressing furnace 100 reaches- 0.06MPa to -0.08MPa.In other embodiments, the inert gas can also be helium.
In the present embodiment, by using the method for furnace cooling, the problem of temperature decrease can be avoided the occurrence of, so as to make It is more solid to form magnesia oxide zinc-oxide alloy 300.
Structure diagram with reference to corresponding to being step S3 in embodiment illustrated in fig. 1 with reference to figure 1 and Fig. 7, Fig. 7 makes described Mold 150 (as shown in Figure 5) is gone naturally after pressing and cooling down, and step S3 is performed, by described 300 (such as Fig. 5 of magnesia oxide zinc-oxide alloy It is shown) it is taken out from the mold 150, obtain magnesia zinc oxide target blankss 400.
In the present embodiment, can by way of dismantling the mold 150, by the magnesia oxide zinc-oxide alloy 300 from It is taken out in the mold 150.
It should be noted that after the magnesia oxide zinc-oxide alloy 300 is taken out from the mold 150, described in acquisition The step of magnesia zinc oxide target blankss 400, further includes:Wire cutting technology is carried out to the magnesia oxide zinc-oxide alloy 300, is formed The initial target blankss of magnesia zinc oxide;Grinding is carried out to the initial target blankss of the magnesia zinc oxide, forms the oxidation magnesia Change zinc target blankss 400.
According to the target size of magnesia zinc oxide target blankss 400 formed, using the wire cutting technology to the oxygen Change magnesium oxide zinc-oxide alloy 300 to be split, and by the grinding, make the size of the magnesia zinc oxide target blankss 400 Meet process requirements with pattern, improve the presentation quality and appearance uniformity of the magnesia zinc oxide target blankss 400.
The magnesia zinc oxide target blankss 400 for manufacturing sputtering target material, therefore also need to be welded with backboard, splash by formation It shoots at the target material.
In the present embodiment, it will thus provide zinc oxide, magnesia mixed-powder 103 it is (as shown in Figure 3) be packed into mold 150 (such as Shown in Fig. 5) after, hot-pressing sintering technique is carried out to the zinc oxide, magnesia mixed-powder 103, magnesia zinc oxide is formed and closes Golden 300 (as shown in Figure 5);After the magnesia oxide zinc-oxide alloy 300 is taken out from the mold 150, oxidation magnesia is obtained Change zinc target blankss 400 (as shown in Figure 7).Compared to normal pressure-sintered or cold pressing forming process scheme, scheme of the present invention can carry Height forms the consistency of magnesia zinc oxide target blankss 400 and microhomogeneity, the reduction magnesia zinc oxide target The cracked probability of base 400, allow the magnesia zinc oxide target blankss 400 consistency reach 98% and more than, and make The magnesia zinc oxide target blankss 400 have uniform color and luster, so as to improve the property of formed magnesia zinc oxide target blankss 400 Can, make the magnesia zinc oxide target blankss 400 that there is stable physical property and meet sputtering target material performance requirement.
Although oneself is disclosed in the preferred embodiments as above the present invention, present invention is not limited to this.Any art technology Personnel without departing from the spirit and scope of the present invention, can make various changes or modifications, therefore protection scope of the present invention should When being subject to claim limited range.

Claims (21)

1. a kind of manufacturing method of magnesia zinc oxide target blankss, which is characterized in that including:
Zinc oxide, magnesia mixed-powder are provided;
After the zinc oxide, magnesia mixed-powder are packed into mold, hot pressing is carried out to the zinc oxide, magnesia mixed-powder Sintering process forms magnesia oxide zinc-oxide alloy;
The magnesia oxide zinc-oxide alloy from the mold is taken out, obtains magnesia zinc oxide target blankss.
2. the manufacturing method of magnesia zinc oxide target blankss as described in claim 1, which is characterized in that the hot-pressing sintering technique The step of include:Mold equipped with the zinc oxide, magnesia mixed-powder is placed in hot pressing furnace;
The hot pressing furnace is carried out to be evacuated to predetermined vacuum value;
After the hot pressing furnace reaches the predetermined vacuum value, hot pressed sintering is carried out to the zinc oxide, magnesia mixed-powder.
3. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 2, which is characterized in that the predetermined vacuum value is small In 100Pa.
4. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 2, which is characterized in that the zinc oxide, oxygen Change the step of magnesium mixed-powder carries out hot pressed sintering to include:The first heating behaviour is carried out to the hot pressing furnace with the first heating rate Make, the hot pressing furnace is made to be warming up to the first preset temperature, and in the first heating operating process, keep the mold by Pressure be first pressure value;
After the hot pressing furnace is warming up to first preset temperature, the second heating carries out the hot pressing furnace with the second heating rate Operation, makes the hot pressing furnace be warming up to the second preset temperature;
After the hot pressing furnace is warming up to second preset temperature, heat preservation operation is carried out to the mold;
After the heat preservation operation, boost operations are carried out to the mold with default rate of pressure rise, until the mold by Compressive load per unit area reach second pressure value;
Under second preset temperature and second pressure value, heat-insulation pressure keeping operation is carried out to the mold.
5. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 4, which is characterized in that the first heating rate For 5 degrees celsius/minutes to 10 degrees celsius/minutes, first preset temperature is 900 degrees Celsius to 1000 degrees Celsius.
6. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 4, which is characterized in that the first pressure value is 10 tons to 15 tons.
7. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 4, which is characterized in that second heating rate For 3 degrees celsius/minutes to 5 degrees celsius/minutes, second preset temperature is 1200 degrees Celsius to 1500 degrees Celsius.
8. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 4, which is characterized in that protected to the mold In the step of temperature operation, soaking time is 1 hour to 2 hours.
9. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 4, which is characterized in that the default rate of pressure rise For 1 tons minute, 5 tons minute, the second pressure value is 20MPa to 30MPa.
10. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 4, which is characterized in that carried out to the mold In the step of heat-insulation pressure keeping operates, the time of heat-insulation pressure keeping is 30 minutes to 60 minutes.
11. the manufacturing method of magnesia zinc oxide target blankss as described in claim 1, which is characterized in that provide the zinc oxide, The step of magnesia mixed-powder, includes:Zinc oxide powder and magnesium oxide powder are provided;Using mixed powder machine to the oxide powder and zinc End and magnesium oxide powder carry out mechanical mixture, form zinc oxide, magnesia mixed-powder.
12. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 11, which is characterized in that the Zinc oxide powder Mass ratio with magnesium oxide powder is 77:23 to 97:3.
13. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 11, which is characterized in that the mechanical mixture Technique is wet blending process;
In the step of carrying out mechanical mixture to the Zinc oxide powder and magnesium oxide powder using mixed powder machine, into the mixed powder machine Solvent is added in, mixed slurry is formed after the Zinc oxide powder and magnesium oxide powder mixing;
After the mechanical mixture, the manufacturing method further includes:The mixed slurry is placed in drying box, place is dried Reason, and screening granulation processing is carried out after drying process.
14. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 13, which is characterized in that the solvent is industry Alcohol, pure water or carbon tetrachloride solution.
15. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 13, which is characterized in that using mixed powder machine to institute In the step of stating Zinc oxide powder and magnesium oxide powder progress mechanical mixture, medium ball is added in into the mixed powder machine.
16. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 15, which is characterized in that the medium ball and institute State zinc oxide, the mass ratio of magnesia mixed-powder is 1:1 to 1:3.
17. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 15, which is characterized in that the medium ball includes Two or three in first zirconia ball, the second zirconia ball and third zirconia ball, and first zirconia ball, second The diameter of zirconia ball and third zirconia ball is different.
18. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 17, which is characterized in that first zirconium oxide A diameter of 10 millimeters of ball, a diameter of 20 millimeters of second zirconia ball, a diameter of 30 milli of the third zirconia ball Rice.
19. the manufacturing method of magnesia zinc oxide target blankss as claimed in claim 17, which is characterized in that the medium ball includes First zirconia ball, the second zirconia ball and third zirconia ball, first zirconia ball, the second zirconia ball and third oxygen The mass ratio for changing zirconium ball is 1:1:1 to 1:2:3.
20. the manufacturing method of magnesia zinc oxide target blankss as described in claim 1, which is characterized in that form the magnesia After oxide zinc-oxide alloy, before the magnesia oxide zinc-oxide alloy is taken out from the mold, the manufacturing method further includes:It is right The mold carries out pressure cooling.
21. the manufacturing method of magnesia zinc oxide target blankss as described in claim 1, which is characterized in that by the oxidation magnesia The step of changing after kirsite takes out from the mold, obtaining the magnesia zinc oxide target blankss further includes:To the magnesia Oxide zinc-oxide alloy carries out wire cutting technology, forms the initial target blankss of magnesia zinc oxide;
Grinding is carried out to the initial target blankss of the magnesia zinc oxide, forms the magnesia zinc oxide target blankss.
CN201611245666.9A 2016-12-29 2016-12-29 The manufacturing method of magnesia zinc oxide target blankss Pending CN108249911A (en)

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CN109133910A (en) * 2018-09-13 2019-01-04 先导薄膜材料(广东)有限公司 The production method of ZMO target
CN109133910B (en) * 2018-09-13 2021-07-20 先导薄膜材料(广东)有限公司 Production method of ZMO target material
JPWO2020090867A1 (en) * 2018-10-31 2021-09-16 出光興産株式会社 Sintered body
JP7328246B2 (en) 2018-10-31 2023-08-16 出光興産株式会社 sintered body
CN111375998A (en) * 2020-04-03 2020-07-07 宁波江丰电子材料股份有限公司 Method for controlling thickness uniformity of magnetic target
CN111375998B (en) * 2020-04-03 2022-04-19 宁波江丰电子材料股份有限公司 Method for controlling thickness uniformity of magnetic target
CN112225565A (en) * 2020-10-14 2021-01-15 宁波江丰电子材料股份有限公司 Preparation method of tungsten-silicon target blank
CN112456989A (en) * 2020-12-22 2021-03-09 宁波江丰电子材料股份有限公司 Preparation method of silicon dioxide target blank
CN115141012A (en) * 2022-07-25 2022-10-04 宁波江丰电子材料股份有限公司 Ternary metal oxide ceramic target material and preparation method thereof
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
CN116903349A (en) * 2023-07-13 2023-10-20 宁波江丰电子材料股份有限公司 Preparation method of large-size magnesium oxide target

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Application publication date: 20180706