CN102653470B - Cr2AlC ceramic target and preparation method thereof by vacuum hot pressing - Google Patents
Cr2AlC ceramic target and preparation method thereof by vacuum hot pressing Download PDFInfo
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Abstract
The invention relates to a Cr2AlC ceramic target and a preparation method thereof by vacuum hot pressing, which comprises the following steps: mixing chromium powder, aluminum powder and carbon powder in a mol ratio of 2:(1-1..5):1, and prepressing into a blank; vacuumizing a hot pressing furnace to 10<-1>Pa, heating to 600-650 DEG C at 5-10 DEG C/min, and keeping the temperature for 1-2 hours; heating to 1300-1500 DEG C at 10-20 DEG C/min, pressurizing to 10-30MPa, keeping the temperature and pressure for 2-4 hours, and cooling to 900-1100 DEG C, and relieving the pressure to normal pressure; cooling to room temperature to obtain the blank; and after machining and electromachining, cleaning, and drying to obtain the high-purity high-single-phase-content Cr2AlC ceramic target. The densityof the prepared Cr2AlC ceramic target is up to higher than 97%, the Cr2AlC compound phase content is up to 98-99%, the oxygen content of the target is low, the target quality satisfies the coating preparation requirement, the cost is low, and thus, the invention is suitable for industrial production of large-size Cr2AlC ceramic targets.
Description
Technical field
The present invention relates to a kind of preparation of target materials method for high temperature coating, be specially a kind of chromium two aluminium-carbon ceramic target and vacuum hot-pressing preparation method thereofs thereof, belong to the ceramic target preparing technical field.
Background technology
Pottery is indispensable a kind of material in human lives and the production, and its range of application spreads all over the every field of national economy.As everyone knows, the chemical bonds of ceramic material generally is ionic bond and covalent bond, this chemical bond have very strong directionality and very high in conjunction with can, therefore, the performance of ceramic material shows as generally that hardness is large, fusing point is high, chemical stability is high.Ceramic material shows as intrinsic fragility, and general being difficult to produces plastic deformation, thereby limited its application.Although the ceramic research person has done a lot of work aspect ceramic toughening, very high, the complex process of the general cost of these methods.
In recent years, a class had the double carbide of layer structure and the study hotspot that nitride becomes domestic and international researcher.The characteristics of this compounds metallic bond, covalent bond coexistence, make it have the performance of metal, as good heat conductivility and electric conductivity are at high temperature arranged, lower Vickers hardness and modulus of shearing are arranged, very good thermal shock resistance, can as metal, carry out machining and electric machining, and at high temperature have plasticity; Simultaneously it also has the performance of pottery, and higher yield strength is arranged, high-melting-point, high thermal stability and good anti-oxidant and decay resistance and higher elastic modelling quantity.These special performances have overcome the limitation of traditional ceramics material, so that this class material is with a wide range of applications.Chromium two aluminium carbon are typically a kind of in this compounds, compare similar compound, have better antioxygenic property.
The performance characteristics of chromium two aluminium carbon has a good application prospect it aspect high temperature coating.According to the people's such as M.Baben result of study, because Cr
2AlC can generate fine and close Cr in oxidizing process
2O
3, Al
2O
3Oxide layer can effectively stop oxygen to the coating diffusion inside in case form the oxide of these two kinds of densifications, and other ternary layered compounds of comparing have better antioxygenic property.The people such as Sweden Uppsala University and University West researcher Jenny Frodelius and Janna Jiang select the Ti in such ternary compound
2The AlC powder, adopt supersonic flame spraying method to prepare even, fine and close coating, and with delivered several pieces of research papers in 2009～2010, relate generally to the aspects such as coating preparation, performance study, and compare with the performance of traditional NiCrAlY buffer layer material.The property that such material metal, pottery have concurrently is having a good application prospect it aspect the high temperature coating buffer layer material.The method that tradition prepares high temperature coating is generally electron beam gas phase physical deposition, magnetron sputtering etc., and these preparation methods all with the raw material of target as the preparation coating, therefore prepare high-purity, large scale chromium two aluminium carbon targets are very important to the application of this material.
Chinese invention patent (CN200610028833.4) discloses and has a kind ofly prepared Cr with molten-salt growth method
2The method of AlC powder, but Cr contained in the powder of preparation
7C
3And Cr
2The impurity phases such as Al, and employed salt post-processed is improper easily to environment in the preparation process; Chinese invention patent (CN200810105008.9) discloses the synthetic Cr of a kind of pressureless sintering
2The method of AlC ceramic powder, but consider in the pressureless sintering preparation process that 660 degree left and right sides aluminium will flow in a large number, and loss is serious, and the powder agglomeration for preparing is serious, the follow-up a large amount of power of process need consumption, the energy that is broken for powder.
Exploitation chromium two alumina-carbon materials need the chromium two aluminium carbon targets of high-purity high single-phase content in the application of coatings art, thereby for the follow-up coating that obtains this compound provides raw material, the preparation of the present invention is mainly high-purity, high single-phase content chromium two aluminium carbon targets.
Summary of the invention
One of the object of the invention is to provide a kind of high-purity, high single-phase content, high-compactness chromium two aluminium carbon targets.According to the target of the present invention's preparation, all can satisfy the requirement of coating preparation to target aspect purity, single-phase content, the density, simultaneously owing to the nearly final molding of powder metallurgy, the subsequent process steps that needs is few, and cost is lower generally.
In order to realize above-mentioned purpose of the present invention, the technical scheme of employing is:
A kind of chromium two aluminium-carbon ceramic targets is characterized in that: the single-phase content of chromium two aluminium carbon is 98%～99% in the described ceramic target.The chemical formula of chromium two aluminium carbon is Cr
2AlC, its atomic percent consists of: 50% chromium, 25% chromium, 25% carbon.
A kind of preferred version is characterized in that: the total content of host element chromium, aluminium and carbon is greater than 99.9% in the described ceramic target.
A kind of preferred version is characterized in that: described ceramic target density reaches 5.1g/cm
3, the relative density of target is greater than 97%.
Another object of the present invention provides the preparation method of the chromium two aluminium carbon targets of a kind of high-purity, high single-phase content, high-compactness.The present invention adopts the vacuum hotpressing method, has moderate cost, and the target density is higher.
In order to realize above-mentioned purpose of the present invention, the technical scheme of employing is:
A kind of vacuum hot-pressing preparation method thereof of chromium two aluminium-carbon ceramic targets may further comprise the steps:
(1) with chromium powder, aluminium powder and carbon dust according to mol ratio 2:(1 ~ 1.5): 1 the batching after, carry out mechanical mixture, the material powder that obtains mixing;
(2) the resulting material powder of step (1) is packed in the graphite jig of certain size, carry out the precompressed base, after the precompressed graphite jig is moved in the vacuum sintering funace;
(3) hot pressing furnace vacuumizes with mechanical pump first, is evacuated to 10 with lobe pump again
-1Pa, then the programming rate with 5 ~ 10 ℃/min is warmed up to 600 ~ 650 ℃, is incubated 1 ~ 2 hour, does not pressurize;
(4) heat up with the programming rate of 10 ~ 20 ℃/min subsequently, and begin continuous axial pressure, when temperature is increased to 1300 ~ 1500 ℃, when axial compressive force reaches 10～30MPa, the beginning heat-insulation pressure keeping, heat-insulation pressure keeping is after 2 ~ 4 hours, close heating power supply and begin cooling, drop to 900-1100 ℃ Deng furnace body temperature, gradually slowly pressure release is to normal pressure;
(5) after hot pressing furnace is cooled to room temperature fully, takes out graphite jig and obtain chromium two aluminium carbon target blanks;
(6) chromium two aluminium carbon target blanks are carried out machining and electric machining, then clean, dry, obtain high-purity high single-phase content chromium two aluminium-carbon ceramic targets.
A kind of preferred version is characterized in that: in the step (1), the purity of described chromium powder, aluminium powder and carbon dust is all greater than 99.9%, and particle diameter is all less than 20 μ m.
A kind of preferred version is characterized in that: in the step (1), and the excessive 10～30at% of aluminium powder in the proportioning of raw material, namely chromium powder, aluminium powder and carbon dust are according to mol ratio 2:(1.1 ~ 1.3): 1 batching.
A kind of preferred version is characterized in that: in the step (1), described mechanical mixture is mixed for ball milling in the ball grinder that raw material is packed into, and the ball milling incorporation time is 10～15 hours.
A kind of preferred version is characterized in that: in the step (2), described precompressed adopts jack to carry out precompressed, and preload pressure is 1～3MPa.
A kind of preferred version is characterized in that: in the step (6), described machining is grinding, and electric machining is the line cutting processing; Described cleaning is carried out Ultrasonic Cleaning for target is put into the pure water that contains cleaning agent, cleans after 1～2 hour, changes pure water and carries out Ultrasonic Cleaning 1～2 hour again; After cleaning target is put into drying in oven, obtain at last preparing the target that coating is used.
Preparation of target materials of the present invention is take high-purity chromium powder, aluminium powder and carbon dust as raw material, consider the actual conditions of aluminium element volatilization in the raw material proportioning, make the excessive 0 ~ 50at% of aluminium powder, be that chromium powder, aluminium powder and carbon dust are according to mol ratio 2:(1 ~ 1.5): 1 batching, adopt the vacuum hot-pressing process of HTHP to prepare chromium two aluminium-carbon ceramic targets.Do not add any additive in the hot-pressing sintering technique process, adopt the two-part heating in the hot pressing, low-temperature zone slowly heating has prevented the rapid melting of aluminium, and makes the composition diffusion evenly; The high temperature section Fast Heating has prevented that the too fast of crystal grain from growing up, and the chromium two aluminium carbon targets of preparation have homogeneous chemical composition, the characteristics that grain size is moderate.
The present invention has following outstanding feature:
1, adopt vacuum heating-press sintering technique to prepare chromium two aluminium-carbon ceramic targets, be conducive to obtain high, the larger-size ceramic target of higher, the single-phase content of density, with respect to traditional pressureless sintering method, the chromium two aluminium-carbon ceramic targets of preparation all have very large advantage on density and intensity.
2, the hot pressing process using segmented temperature-rising method, adopting the programming rate of 5 ~ 10 ℃/min slowly to heat up below 600 ℃, and at 600～650 ℃ of low-temperature zone employing with no pressure vacuum heat-preservings, effectively prevent aluminium flowing in temperature-rise period, make aluminium that time enough diffusion be arranged and make the base substrate internal component even, mold integral is heated evenly, and the target that obtains composition and even density in the follow-up hot pressing is given security.
3, the pressurize technique in subsequently high temperature section intensification, pressing technology and the temperature-fall period can further improve the density of target, and preparation temperature and temperature retention time are moderate, have avoided the target crystalline grains over-dimension to grow up.This technique can reach the requirement of high-compactness target, has also avoided the excessive grain of target to grow up simultaneously.
4, consider the partial loss of aluminium in the temperature-rise period during this method batch mixing in the raw material proportioning, added the excess of aluminum raw material, can guarantee the chromium two aluminium carbon target complete reactions that prepare, avoided the dephasign generation, improve the single-phase content of target.
The chromium two aluminium-carbon ceramic target densityes of the present invention's preparation reach more than 97%, the single-phase content of chromium two aluminium carbon reaches 98% ~ 99%, and the oxygen content of target is low, and the target quality satisfies coating and prepares requirement, this preparation method's cost is lower, is fit to large scale chromium two aluminium-carbon ceramic target suitability for industrialized production.
The present invention will be further described below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is for adopting the chromium two aluminium carbon (Cr of the inventive method preparation
2AlC) X ray of target is composed fitted figure entirely.
The specific embodiment
Embodiment 1
Take by weighing Cr powder 104 grams, Al powder 32.4 grams, C powder 12 grams, the purity of chromium powder, aluminium powder and carbon dust is all greater than 99.9%, and particle diameter all less than 20 μ m, is put into ball grinder, and adds 300 gram agate balls, ball milling 12 hours.Material powder is put into graphite jig, adopts the jack pair raw material to carry out axial precompressed, and preload pressure is 2MPa, after the precompressed graphite jig is moved in the vacuum sintering funace.Hot pressing furnace is evacuated to the certain vacuum degree, is evacuated to 10 with lobe pump again with mechanical pump first
-1Pa, then the programming rate with 5 ℃/min is warmed up to 630 ℃, is incubated 2 hours, does not pressurize; Speed with 10 ℃/min heats up, progressively pressurizes subsequently, rises to 1350 ℃ of temperature, and pressure is 20MPa, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and after temperature reached 1100 ℃, pressure release was cooled off 10 hours, and furnace temperature drops to room temperature, goes out blank.Blank is carried out grinding and line cutting processing; Target after the processing is put into the pure water that contains oil-removing cleaning agent, carries out Ultrasonic Cleaning, cleans after 1 hour, changes pure water and again carries out Ultrasonic Cleaning 1 hour; Target after cleaning is put into the vacuum drying chamber oven dry, obtains preparing the high single-phase content chromium two aluminium-carbon ceramic targets that coating is used.The density of target reaches 5.1g/cm
3, relative density reaches 97.6%, and target is carried out the analysis of XRD phase content, and wherein chromium two aluminum-carbon ternary phase contents reach 98.4%.
Fig. 1 is the chromium two aluminium carbon target XRD phase content analysis results of present embodiment preparation.To carrying out match in the full spectral limit of XRD spectral line, quantitatively calculate through phase content, obtain adopting that the single-phase content of chromium two aluminium carbon reaches 98.4% in the target of the method preparation.
Embodiment 2
Take by weighing Cr powder 156 grams, Al powder 48 grams, C powder 18 grams, put into ball grinder, and add 300 gram agate balls, ball milling 13 hours.Material powder is put into graphite jig, adopts the jack pair raw material to carry out axial precompressed, and preload pressure is 2MPa, after the precompressed graphite jig is moved in the vacuum sintering funace.Hot pressing furnace successively vacuumizes 10 with mechanical pump, lobe pump
-1Pa, then the programming rate with 5 ℃/min is warmed up to 630 ℃, is incubated 2 hours; Speed with 10 ℃/min heats up, progressively pressurizes subsequently, rises to 1400 ℃ of temperature, and pressure is 20MPa, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and after temperature reached 1000 ℃, pressure release was cooled off 10 hours, and furnace temperature drops to room temperature, goes out blank.Blank is carried out machining and electric machining, and target is put into the pure water that contains oil-removing cleaning agent after the processing, carries out Ultrasonic Cleaning, cleans after 1 hour, changes pure water and again carries out Ultrasonic Cleaning 1 hour; Target after cleaning is put into the vacuum drying chamber oven dry, obtains preparing the high single-phase content chromium two aluminium-carbon ceramic targets that coating is used.The density of target reaches 5.12g/cm
3, relative density reaches 97.9%, and target is carried out the analysis of XRD phase content, and its chromium two aluminium carbon phase contents reach 98.2%.
Embodiment 3
Take by weighing Cr powder 312 grams, Al powder 100 grams, C powder 36 grams, put into ball grinder, and add 600 gram agate balls, ball milling 15 hours.Material powder is put into graphite jig, adopts the jack pair raw material to carry out axial precompressed, and preload pressure is 3MPa, after the precompressed graphite jig is moved in the vacuum sintering funace.Hot pressing furnace successively vacuumizes 10 with mechanical pump, lobe pump
-1Pa, then the programming rate with 5 ℃/min is warmed up to 650 ℃, is incubated 2 hours; Speed with 10 ℃/min heats up, progressively pressurizes subsequently, rises to 1500 ℃ of temperature, and pressure is 30MPa, and heat-insulation pressure keeping was closed heating power supply after 2 hours, begins cooling, and after temperature reached 1100 ℃, pressure release was cooled off 10 hours, and furnace temperature drops to room temperature, goes out blank.Blank is carried out machining and electric machining, and target is put into the pure water that contains oil-removing cleaning agent after the processing, carries out Ultrasonic Cleaning, cleans after 2 hours, changes pure water and again carries out Ultrasonic Cleaning 2 hours; Target after cleaning is put into the vacuum drying chamber oven dry, obtains preparing the high single-phase content chromium two aluminium-carbon ceramic targets that coating is used.The density of target reaches 5.09g/cm
3, relative density reaches 97.3%, and target is carried out the analysis of XRD phase content, and its chromium two aluminium carbon phase contents reach 98.1%.
Embodiment 4
Take by weighing Cr powder 208 grams, Al powder 70 grams, C powder 24 grams, put into ball grinder, and add 600 gram agate balls, ball milling 13 hours.Material powder is put into graphite jig, adopts the jack pair raw material to carry out axial precompressed, and preload pressure is 1MPa, after the precompressed graphite jig is moved in the vacuum sintering funace.Hot pressing furnace successively vacuumizes 10 with mechanical pump, lobe pump
-1Pa, then the programming rate with 10 ℃/min is warmed up to 620 ℃, is incubated 1 hour; Speed with 15 ℃/min heats up, progressively pressurizes subsequently, rises to 1450 ℃ of temperature, and pressure is 10MPa, and heat-insulation pressure keeping was closed heating power supply after 4 hours, begins cooling, and after temperature reached 900 ℃, pressure release was cooled off 12 hours, and furnace temperature drops to room temperature, goes out blank.Blank is carried out machining and electric machining, and target is put into the pure water that contains oil-removing cleaning agent after the processing, carries out Ultrasonic Cleaning, cleans after 1 hour, changes pure water and again carries out Ultrasonic Cleaning 2 hours; Target after cleaning is put into the vacuum drying chamber oven dry, obtains preparing the high single-phase content chromium two aluminium-carbon ceramic targets that coating is used.The density of target reaches 5.20g/cm
3, relative density reaches 99.4%, and target is carried out the analysis of XRD phase content, and its chromium two aluminium carbon phase contents reach 99%.
Embodiment 5
Take by weighing Cr powder 130 grams, Al powder 40 grams, C powder 15 grams, put into ball grinder, and add 400 gram agate balls, ball milling 10 hours.Material powder is put into graphite jig, adopts the jack pair raw material to carry out axial precompressed, and preload pressure is 2MPa, after the precompressed graphite jig is moved in the vacuum sintering funace.Hot pressing furnace successively vacuumizes 10 with mechanical pump, lobe pump
-1Pa, then the programming rate with 10 ℃/min is warmed up to 600 ℃, is incubated 1 hour; Speed with 20 ℃/min heats up, progressively pressurizes subsequently, rises to 1300 ℃ of temperature, and pressure is 20MPa, and heat-insulation pressure keeping was closed heating power supply after 3 hours, begins cooling, and after temperature reached 1000 ℃, pressure release was cooled off 10 hours, and furnace temperature drops to room temperature, goes out blank.Blank is carried out machining and electric machining, and target is put into the pure water that contains oil-removing cleaning agent after the processing, carries out Ultrasonic Cleaning, cleans after 2 hours, changes pure water and again carries out Ultrasonic Cleaning 1 hour; Target after cleaning is put into the vacuum drying chamber oven dry, obtains preparing the high single-phase content chromium two aluminium-carbon ceramic targets that coating is used.The density of target reaches 5.17g/cm
3, relative density reaches 98.85%, and target is carried out the analysis of XRD phase content, and its chromium two aluminium carbon phase contents reach 98.7%.
Claims (5)
1. the vacuum hot-pressing preparation method thereof of chromium two aluminium-carbon ceramic targets may further comprise the steps:
(1) with chromium powder, aluminium powder and carbon dust according to mol ratio 2:(1～1.5): 1 the batching after, carry out mechanical mixture, the material powder that obtains mixing, the purity of described chromium powder, aluminium powder and carbon dust is all greater than 99.9%, particle diameter is all less than 20 μ m;
(2) the resulting material powder of step (1) is packed in the graphite jig, carry out the precompressed base, after the precompressed graphite jig is moved in the vacuum sintering funace;
(3) hot pressing furnace vacuumizes with mechanical pump first, is evacuated to 10 with lobe pump again
-1Pa, then the programming rate with 5～10 ℃/min is warmed up to 600～650 ℃, is incubated 1～2 hour, does not pressurize;
(4) subsequently with the programming rate of 10～20 ℃/min, and begin continuous axial pressure, when temperature is increased to 1300～1500 ℃, when axial compressive force reaches 10～30MPa, the beginning heat-insulation pressure keeping, heat-insulation pressure keeping is after 2～4 hours, close heating power supply and begin cooling, drop to 900-1100 ℃ Deng furnace body temperature, gradually slowly pressure release is to normal pressure;
(5) after hot pressing furnace is cooled to room temperature fully, takes out graphite jig and obtain chromium two aluminium carbon target blanks;
(6) chromium two aluminium carbon target blanks are carried out machining and electric machining, then clean, dry, obtain high-purity high single-phase content chromium two aluminium-carbon ceramic targets, the single-phase content of chromium two aluminium carbon reaches 98%～99% in the described ceramic target, the total content of host element chromium, aluminium and carbon is greater than 99.9% in the described ceramic target, and described ceramic target density reaches 5.1g/cm
3, the relative density of target is greater than 97%.
2. the vacuum hot-pressing preparation method thereof of chromium two aluminium-carbon ceramic targets according to claim 1 is characterized in that: the excessive 10～30at% of aluminium powder in the described material powder.
3. the vacuum hot-pressing preparation method thereof of chromium two aluminium-carbon ceramic targets according to claim 1 is characterized in that: described mechanical mixture is mixed for ball milling in the ball grinder that raw material is packed into, and the ball milling incorporation time is 10～15 hours.
4. the vacuum hot-pressing preparation method thereof of chromium two aluminium-carbon ceramic targets according to claim 1 is characterized in that: described precompressed adopts jack to carry out precompressed, and preload pressure is 1～3MPa.
5. the vacuum hot-pressing preparation method thereof of chromium two aluminium-carbon ceramic targets according to claim 1, it is characterized in that: described machining is grinding, electric machining is the line cutting processing; Described cleaning is carried out Ultrasonic Cleaning for target is put into the pure water that contains oil-removing cleaning agent, cleans after 1～2 hour, changes pure water and carries out Ultrasonic Cleaning 1～2 hour again; After cleaning target is put into drying in oven, obtain at last preparing the target that coating is used.
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| CN102899612B (en) * | 2012-09-21 | 2014-03-26 | 中国科学院金属研究所 | Method for preparing high-temperature protective coating with Cr2AlC as main phase by employing multi-arc ion plating |
| CN110776311B (en) * | 2019-11-06 | 2021-07-30 | 常州大学 | Method for preparing perovskite type composite oxide high-entropy ceramic by hot-pressing sintering |
| CN111320478B (en) * | 2020-03-27 | 2022-02-11 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of carbon-silicon ceramic target material |
| CN112111663A (en) * | 2020-08-06 | 2020-12-22 | 西安交通大学 | High-strength MAB ceramic compact block and preparation method thereof |
| CN115745603B (en) * | 2022-10-17 | 2023-08-29 | 河北东同光电科技有限公司 | Preparation method of large-size high-performance niobium oxide target |
| CN115894034A (en) * | 2022-12-08 | 2023-04-04 | 北京航空航天大学 | Preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application |
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| CN1743480A (en) * | 2005-09-29 | 2006-03-08 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of aluminium-carbon-dichromium block material |
| CN1884064A (en) * | 2006-07-12 | 2006-12-27 | 中国科学院上海硅酸盐研究所 | Method for preparing Cr2AlC by molten salt process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1743480A (en) * | 2005-09-29 | 2006-03-08 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of aluminium-carbon-dichromium block material |
| CN1884064A (en) * | 2006-07-12 | 2006-12-27 | 中国科学院上海硅酸盐研究所 | Method for preparing Cr2AlC by molten salt process |
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