CN109439990A - A kind of preparation process of high-compactness high-content molybdenum niobium alloy target - Google Patents
A kind of preparation process of high-compactness high-content molybdenum niobium alloy target Download PDFInfo
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- CN109439990A CN109439990A CN201811638273.3A CN201811638273A CN109439990A CN 109439990 A CN109439990 A CN 109439990A CN 201811638273 A CN201811638273 A CN 201811638273A CN 109439990 A CN109439990 A CN 109439990A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of preparation process of high-compactness high-content molybdenum niobium alloy target, the raw material of the preparation process are made of the following components measured by mass percentage: niobium powder 5%-15%, surplus are molybdenum powder；The a part for weighing the niobium powder is produced to obtain secondary hydrogenated niobium by the hydrogenation process of niobium；The mass ratio of the secondary hydrogenated niobium and the raw material is 0.1:100-3:100, and the secondary hydrogenated niobium is in powdered, grain diameter D90≤50 μm.The present invention utilizes the activation of secondary hydrogenated niobium, and the technological parameter by producing secondary hydrogenated niobium, and high-compactness high-content molybdenum niobium alloy sputtering target material is directly prepared using powder metallurgical technique.
Description
Technical field
The invention belongs to rare metal technical fields, and in particular to a kind of high-compactness high-content for adding secondary hydrogenated niobium
The preparation process of molybdenum niobium alloy target.
Background technique
Sputtering is the ion generated using ion source, accelerates to be gathered into the Fast ion flow bombardment surface of solids in a vacuum,
So that the atom of the surface of solids is left target and is deposited on substrate surface, thus form nanometer to micron film, the solid bombarded
Referred to as sputtering target material.Sputter coating is integrated circuit, flat-panel monitor (including liquid crystal display and touch screen etc.), the film sun
Energy battery and light emitting diode (LED) etc. fields prepare the basic means of function film, and sputtering target material just becomes these fields
Indispensable basic material.
With the continuous improvement to electronic product comprehensive performance and use environment requirement, performance to sputtering target material it is also proposed that
Increasingly higher demands.Although molybdenum is the electrode and wiring material of ideal flat-panel screens, thin-film solar cells
And the barrier material of semiconductor, but in the application, discovery molybdenum is in corrosion resistance (discoloration) and adherence (removing of film) side
There are still problems in face.Research and practice have shown that, the alloying elements such as niobium are added in molybdenum titanium sputtering target, sputtered film after sputtering can be made
The various performances such as specific impedance, stress, corrosion resistance reach balanced, more and more favored.
Molybdenum niobium alloy can be made by melt casting process, i.e., by the molybdenum centainly matched, niobium raw material melting, then by alloy
Melt is cast in mold, obtains ingot casting, then thermally treated, forging, extruding and rolling etc. and target is made.It is lacked existing for this technique
It is trapped in, the gained ingot casting shrinkage cavity the problems such as, and ingot casting coarse grains, the problems such as homogeneity of ingredients is poor, and process equipment condition
It is required that high.
Molybdenum niobium alloy can also be made by powder metallurgical technique.Presently, there are a variety of specific works for powder metallurgical technique
Skill, the first technique are after mixing a certain amount of molybdenum powder and niobium powder, and repressed forming, vacuum-sintering obtain ingot casting, this technique
The shortcomings that be that the oxygen impurities volatilization in molybdenum powder and niobium powder is difficult, prevent sintering densification, gained ingot casting relative density only has 80-
89%, its improvement version technique is forged again to gained ingot casting or rolling processing, but complex process, yield rate be not also high；The
Two kinds of techniques are to mix a certain amount of molybdenum powder and niobium powder, carry out vacuum hotpressing after repressed forming or hot isostatic pressing acquires casting
Ingot, gained ingot casting relative density can achieve 90-97%, but due to needing using graphite jig, and the device is complicated, expensive, and
Easy carburizing；The third technique mixes a certain amount of molybdenum powder and niobium powder, is sintered after repressed forming, then cast through hot isostatic pressing
Ingot, obtaining ingot casting relative density can reach 98% or more, and disadvantage is long flow path, complicated for operation, at high cost.
Patent " a kind of preparation process of high-compactness high-content molybdenum niobium alloy target " (CN105648407A), using addition
The mode of zircoium hydride prepares the molybdenum niobium alloy that relative density is 98% or more, but since addition new component zircoium hydride enters
In molybdenum niobium alloy, be tantamount to addition impurity, direct result is exactly obtained molybdenum niobium alloy content reduction, moreover, zirconium fusing point compared with
Molybdenum is 770 DEG C low, and 1143 DEG C low compared with niobium, and metal zirconium easily forms zirconium oxide on surface, and these properties will lead to molybdenum niobium alloy
Quality reduces.
Moreover, major impurity is carbon and oxygen in molybdenum powder and niobium powder, the product of different manufacturers production or even same producer are produced
Identical product different batches between both impurity generally also can difference, this needs a kind of substance (can be mixture) different
Activity function, zircoium hydride is a kind of single substance, and performance is single, in practice, there is certain limitation.
Currently, metallurgical technology generally all has metal compactionization and purification dual purpose, in particular by vaccum sintering process；
Powder metallurgical technique has many advantages, such as that aplitic texture is uniform, saves material, high production efficiency, if can be adopted by technical measures
The molybdenum niobium alloy target of high-compactness is directly prepared with conventional powder metallurgical technique, can both improve the relatively close of molybdenum niobium alloy target
Degree, and content can be improved, to satisfactorily reach the dual purpose of metallurgical technology, by the meaning with important reality.
Summary of the invention
Based on the deficiencies of the prior art, the present invention provides a kind of preparation works of high-compactness high-content molybdenum niobium alloy target
Skill obtains secondary hydrogenated niobium by a part to niobium powder in raw material by hydrogenation process, is then added to the compacting of molybdenum niobium alloy
In base, with the molybdenum niobium alloy target of achieve the purpose that get both high-compactness and high-content.
The object of the present invention is achieved like this:
A kind of preparation process of high-compactness high-content molybdenum niobium alloy target, the raw material of the preparation process are by pressing quality
The following components of percentage scale forms: niobium powder 5%-15%, surplus are molybdenum powder；The a part for weighing the niobium powder, passes through niobium
Hydrogenation process produce to obtain secondary hydrogenated niobium；The mass ratio of the secondary hydrogenated niobium and the raw material is 0.1:100-3:
100, the secondary hydrogenated niobium is in powdered, grain diameter D90≤50μm。
Preferably, the preparation process the following steps are included:
A) it produces secondary hydrogenated niobium step: will be hydrogenated in a part merging hydrogenation furnace of the niobium powder, in primary hydrogenation temperature
Degree is lower to react 15min-120min, and a hydrogenated niobium is made, crushes after a hydrogenated niobium is cooled to room temperature, is placed in again
Hydrogenation, reacts 60min-120min under secondary hydrogenation temperature in hydrogenation furnace, and secondary hydrogenated niobium is made, and crushes the secondary hydrogenation
Niobium is to grain diameter D90≤50μm。
B) mixed grinding step: weigh by mass percentage the raw material component and step a made from it is described secondary
Hydrogenated niobium grinds after mixing, obtains mixed-powder；
C) it suppresses base step: by mixed-powder compression moulding under pressure, obtaining compacting base；The base pressure
Power is 150-300 megapascal；
D) vacuum-sintering step: the compacting base is directly subjected to vacuum-sintering, obtains sintered blank；The vacuum-sintering
Holding temperature is 1900-2150 DEG C, and soaking time is 2-8 hours, cools to 120 DEG C after heat preservation with the furnace hereinafter, coming out of the stove again
It is cooled to room temperature；
E) machining steps: the sintered blank is machined out to get the molybdenum niobium alloy target.
Further, a hydrogenation temperature is 400-900 DEG C, and the secondary hydrogenation temperature is 250-500 DEG C.
Preferably, the heating rate of the vacuum-sintering is not more than 10 DEG C/min, and vacuum degree is maintained in temperature-rise period
0.8×10-3To 1.2 × 10-3Between Pa.
The invention has the benefit that
Secondary hydrogenated niobium is made in part niobium powder using the hydrogenation process of niobium, is directly prepared simultaneously using powder metallurgical technique
Have the molybdenum niobium alloy sputtering target material of high-compactness and high-content, simple process and low cost；Due to the hydrogenation work by control niobium
Skill parameter controls the proportion (i.e. NbH0.3 and NbH0.7) of two kinds of hydrogenated niobiums in secondary hydrogenated niobium, adjusts the work of secondary hydrogenated niobium
Change performance, overcomes influence of the material quality variation to finished product quality, final product quality is enable to maintain one compared with Gao Shui
On flat.Obtained molybdenum niobium alloy target can be applied to the preparation of the function films such as touch screen thin film electrode layer.
Detailed description of the invention
Fig. 1 is the process flow chart of the preparation process of high-compactness high-content molybdenum niobium alloy target of the invention.
Specific embodiment
Below by way of preferred embodiment, the present invention is described in more detail, but protection scope of the present invention is not limited to
This.
Raw materials of the embodiment of the present invention are commercial product.
Tables 1 and 2 is manufacturer and the specifications of raw materials parameter of raw materials of the embodiment of the present invention.
Molybdenum powder raw material producer and specification used in 1 embodiment of the present invention of table
Niobium powder raw material producer and specification used in 2 embodiment of the present invention of table
Specific embodiment
A kind of high-compactness high-content molybdenum niobium alloy target, is made of: niobium powder the following components measured by mass percentage
5%, secondary hydrogenated niobium 1.5%, surplus is molybdenum powder, and wherein the 10% of niobium powder is for producing secondary hydrogenated niobium, secondary hydrogen obtained
Changing niobium to be crushed is in powdered, grain diameter D90≤50μm。
Wherein, molybdenum powder, niobium powder are commercial product, and molybdenum powder selects Zhuzhou Jing Zuan hard alloy Co., Ltd, and the trade mark is
The product of FMo-1 or FMo-1；Niobium powder selects Hebei province Nangong City Bo Zhi alloy welding material Co., Ltd, trade mark Titd-Nb's
Product；Secondary hydrogenated niobium is self-control.
The preparation process of above-mentioned high-compactness high-content molybdenum niobium alloy target, comprising the following steps:
A) it produces secondary hydrogenated niobium step: by 400 grams of niobium powder, being divided into 4 parts, every part is placed in hydrogenation in hydrogenation furnace,
30min is reacted at a temperature of 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C respectively, hydrogenated niobium of gained is cooled to room temperature rear ball
Milling is broken to grain diameter D90≤ 60 μm, it is placed in hydrogenation in hydrogenation furnace again, 120min is reacted at a temperature of 300 DEG C and is made secondary
Hydrogenated niobium crushes the hydrogenated niobium to grain diameter D after being cooled to room temperature90≤ 10 μm, 4 parts of different secondary hydrogenated niobiums are made；
B) mixed grinding step: the molybdenum powder of 4 parts of different secondary hydrogenated niobiums and two kinds of specifications, totally eight combinations, each group
It is collectively referred to as taking 22.5g niobium powder, secondary hydrogenated niobium 2.6g, 472.5g molybdenum powder is ground after mixing, is obtained 8 parts of every part of quality and is
The mixed-powder of 500.1g；
C) it suppresses base step: by the compression moulding under 300 megapascal pressures respectively of above-mentioned 8 parts of mixed-powders, obtaining 8 parts
Suppress base；
D) vacuum-sintering step: above-mentioned 8 parts of compactings base is directly subjected to vacuum-sintering, obtains sintered blank；Vacuum-sintering
Holding temperature be 1900-2150 DEG C, soaking time be 8 hours, cool to 120 DEG C after heat preservation with the furnace, then come out and cool down to
Room temperature；Compacting base is sintered in a vacuum furnace, and control heating rate is not more than 6 DEG C/min, and keeps vacuum degree in temperature-rise period little
In 8 × 10-3Pa is warming up to 1950 DEG C and is kept the temperature, and holding stage vacuum degree is 1 × 10-3Pa is hereinafter, vacuum in cooling procedure
Degree is 1 × 10-3Pa is hereinafter, obtain sintered blank；
(4) resulting 8 parts of sintered blanks are machined out, obtain 8 parts of molybdenum niobium alloy targets.
Comparative example
As a comparison, preparing molybdenum niobium alloy target using with identical molybdenum powder above-mentioned in embodiment, niobium powder and preparation process
Material；Wherein, molybdenum powder and the mass ratio of niobium powder are 19:1, do not add secondary hydrogenated niobium, make prepared molybdenum niobium alloy target molybdenum and niobium
Mass ratio it is suitable, obtain two parts of reference examples molybdenum niobium alloy targets.
The density for being measured above-mentioned molybdenum niobium alloy target respectively using drainage is tested and molybdenum niobium alloy target is calculated
Density and relative density (actual density/theoretical density), as shown in table 3.
The density and relative density of 3 molybdenum niobium alloy target of table
| Number | The molybdenum powder trade mark | Hydrogenation temperature/DEG C | Density/MPa | Relative density/% |
| Embodiment | FMo-1 | 400 | 9.76 | 97.4 |
| Embodiment | FMo-1 | 500 | 9.86 | 98.4 |
| Embodiment | FMo-1 | 600 | 9.72 | 97.0 |
| Embodiment | FMo-1 | 700 | 9.62 | 96.0 |
| Embodiment | FMo-2 | 400 | 9.50 | 94.8 |
| Embodiment | FMo-2 | 500 | 9.58 | 95.6 |
| Embodiment | FMo-2 | 600 | 9.63 | 96.1 |
| Embodiment | FMo-2 | 700 | 9.72 | 97.0 |
| Comparative example | FMo-1 | - | 8.80 | 87.8 |
| Comparative example | FMo-2 | - | 8.64 | 86.2 |
From the experimental result of table 3, it is apparent that using preparation process of the invention, the molybdenum added with secondary hydrogenated niobium
The relative density of girl's alloy target material is relatively not added with secondary hydrogenated niobium molybdenum girl's alloy target material and significantly improves, and molybdenum girl produced by the present invention closes
Gold target material relative density can be improved to 98% or more, in simple process and the porosity be significantly reduced, to be made high-densit
The molybdenum girl's alloy target material for spending high-content, help to obtain the sputtered layer of high quality.Also, it is apparent that the quality of molybdenum powder is straight
Influence molybdenum girl's alloy target material relative density obtained is connect, molybdenum girl's alloy of higher relative density can be obtained by adding secondary hydrogenated niobium also
Target, still further it can be seen that, by the control to the hydrogenation temperature of parameter produced in secondary hydrogenated niobium step, can control not
Molybdenum girl alloy target material relative density, which is made, in the molybdenum powder of same specification can pass through control to control the quality of molybdenum girl's alloy target material
These parameters make the molybdenum powder of quality that molybdenum girl's alloy target material of more high quality can also be made, this has spy for production practices
Different meaning is that the direct connection of material quality and product quality can be obstructed to a certain extent, so as to by product
Quality control is in certain level.
The scope of the present invention is not limited by the specific embodiments described, and the embodiment is only used as illustrating of the invention each
The single example of a aspect further includes function equivalent method and component in the scope of the invention.In fact, in addition to as described herein
Outside content, those skilled in the art can easily be grasped referring to description above to a variety of improvement of the invention.The improvement
It also falls within the scope of the appended claims.Every bibliography mentioned above is all included in herein in full as reference.
Claims (4)
1. a kind of preparation process of high-compactness high-content molybdenum niobium alloy target, which is characterized in that the former material of the preparation process
Material is made of the following components measured by mass percentage: niobium powder 5%-15%, surplus are molybdenum powder；Weigh one of the niobium powder
Point, it produces to obtain secondary hydrogenated niobium by niobium hydride technique；The mass ratio of the secondary hydrogenated niobium and the raw material is 0.1:
100-3:100, the secondary hydrogenated niobium are in powdered, grain diameter D90≤50μm。
2. preparation process according to claim 1, which is characterized in that the preparation process the following steps are included:
A) it produces secondary hydrogenated niobium step: will be hydrogenated in a part merging hydrogenation furnace of the niobium powder, under a hydrogenation temperature
15min-120min is reacted, a hydrogenated niobium is made, is crushed after a hydrogenated niobium is cooled to room temperature, again merging hydrogenation
Hydrogenation, reacts 60min-120min under secondary hydrogenation temperature in furnace, and secondary hydrogenated niobium is made, and crushes the secondary hydrogenated niobium extremely
Grain diameter D90≤50μm。
B) mixed grinding step: weigh by mass percentage the raw material component and step a made from the secondary hydrogenation
Niobium grinds after mixing, obtains mixed-powder；
C) it suppresses base step: by mixed-powder compression moulding under pressure, obtaining compacting base；The pressure is
150-300 megapascal；
D) vacuum-sintering step: the compacting base is directly subjected to vacuum-sintering, obtains sintered blank；The heat preservation of the vacuum-sintering
Temperature is 1900-2150 DEG C, and soaking time is 2-8 hours, cools to 120 DEG C after heat preservation with the furnace hereinafter, coming out and cooling down again
To room temperature；
E) machining steps: the sintered blank is machined out to get the molybdenum niobium alloy target.
3. preparation process according to claim 2, which is characterized in that a hydrogenation temperature is 400-900 DEG C, described
Secondary hydrogenation temperature is 250-500 DEG C.
4. preparation process according to claim 2, which is characterized in that the heating rate of the vacuum-sintering is not more than 10
DEG C/min, vacuum degree is maintained at 0.8 × 10 in temperature-rise period-3To 1.2 × 10-3Between Pa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109207941A (en) * | 2017-07-05 | 2019-01-15 | 日立金属株式会社 | MoNb target |
| CN110257784A (en) * | 2019-07-24 | 2019-09-20 | 洛阳高新四丰电子材料有限公司 | A kind of preparation process of high-compactness molybdenum niobium alloy sputtering target material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85109070A (en) * | 1985-12-20 | 1987-06-24 | 北京有色金属研究总院 | The manufacture method of niobium alloy |
| WO2014104178A1 (en) * | 2012-12-27 | 2014-07-03 | 昭和電工株式会社 | Chemical conversion body for niobium capacitor positive electrode, and production method therefor |
| CN104860267A (en) * | 2015-05-12 | 2015-08-26 | 昆明冶金研究院 | Ultrafine hydrogenated niobium powder preparation method |
| CN105648407A (en) * | 2016-01-27 | 2016-06-08 | 郑州大学 | High-density molybdenum-niobium alloy target and preparation process thereof |
-
2018
- 2018-12-29 CN CN201811638273.3A patent/CN109439990A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85109070A (en) * | 1985-12-20 | 1987-06-24 | 北京有色金属研究总院 | The manufacture method of niobium alloy |
| WO2014104178A1 (en) * | 2012-12-27 | 2014-07-03 | 昭和電工株式会社 | Chemical conversion body for niobium capacitor positive electrode, and production method therefor |
| CN104860267A (en) * | 2015-05-12 | 2015-08-26 | 昆明冶金研究院 | Ultrafine hydrogenated niobium powder preparation method |
| CN105648407A (en) * | 2016-01-27 | 2016-06-08 | 郑州大学 | High-density molybdenum-niobium alloy target and preparation process thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109207941A (en) * | 2017-07-05 | 2019-01-15 | 日立金属株式会社 | MoNb target |
| CN109207941B (en) * | 2017-07-05 | 2020-09-29 | 日立金属株式会社 | MoNb target material |
| CN110257784A (en) * | 2019-07-24 | 2019-09-20 | 洛阳高新四丰电子材料有限公司 | A kind of preparation process of high-compactness molybdenum niobium alloy sputtering target material |
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