CN113563098B - ZrB2Composite interlayer connection LaCrO3Process for producing ceramics - Google Patents
ZrB2Composite interlayer connection LaCrO3Process for producing ceramics Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 163
- 239000011229 interlayer Substances 0.000 title claims abstract description 32
- 239000010410 layer Substances 0.000 claims abstract description 92
- 239000000463 material Substances 0.000 claims abstract description 89
- 229910002262 LaCrO3 Inorganic materials 0.000 claims abstract description 83
- 238000000227 grinding Methods 0.000 claims abstract description 81
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910007948 ZrB2 Inorganic materials 0.000 claims abstract description 71
- 238000001035 drying Methods 0.000 claims abstract description 71
- 239000000843 powder Substances 0.000 claims abstract description 61
- 229910017563 LaCrO Inorganic materials 0.000 claims abstract description 57
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 47
- 238000005498 polishing Methods 0.000 claims abstract description 45
- 239000002131 composite material Substances 0.000 claims abstract description 38
- 239000011812 mixed powder Substances 0.000 claims abstract description 30
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 28
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 28
- 235000019441 ethanol Nutrition 0.000 claims abstract description 20
- 238000003825 pressing Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 9
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000000725 suspension Substances 0.000 claims description 14
- 238000006136 alcoholysis reaction Methods 0.000 claims description 7
- 229910003460 diamond Inorganic materials 0.000 claims description 7
- 239000010432 diamond Substances 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims 8
- 239000002245 particle Substances 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- DTDCCPMQHXRFFI-UHFFFAOYSA-N dioxido(dioxo)chromium lanthanum(3+) Chemical compound [La+3].[La+3].[O-][Cr]([O-])(=O)=O.[O-][Cr]([O-])(=O)=O.[O-][Cr]([O-])(=O)=O DTDCCPMQHXRFFI-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
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- C04B2237/04—Ceramic interlayers
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Abstract
The invention discloses a new type of rare earth element (ZrB)2Composite interlayer connection LaCrO3The ceramic process comprises the following steps: preparation of intermediate connection layer powder: reacting ZrB2Fully mixing the powder and Al powder, grinding by taking absolute ethyl alcohol as a grinding medium, drying after grinding, and performing secondary grinding after drying; preparing the intermediate connecting layer round sheet: to intermediate connection layer ZrB2Adding polyvinyl alcohol solution into Al powder, grinding uniformly, drying, and pressing the mixed powder into round slices by a tablet press; LaCrO3Pretreatment of a ceramic base material: firstly to LaCrO3Roughly grinding and polishing the ceramic parent metal, placing the polished ceramic parent metal into an ethanol solution for ultrasonic cleaning, and placing the cleaned ceramic parent metal into an oven for drying; spark plasma sintering connection: LaCrO to be connected3And assembling the ceramic base material and the middle connecting layer round sheet into a graphite mold, and sintering in a discharge plasma sintering furnace. LaCrO prepared by the invention3The highest normal-temperature bending strength of the ceramic connecting piece joint is 23.79MPa, the highest Vickers hardness of the intermediate connecting layer is 7.01GPa, the density is 89.06-99.29%, and the resistivity is 0.03-0.04 m omega/cm3。
Description
Technical Field
The invention relates to the technical field of ceramic connection. In particular to a ZrB2Composite interlayer connection LaCrO3And (3) a ceramic process.
Background
LaCrO3The ceramic isThe functional ceramic has stable chemical property, can be used for a long time in an oxidizing atmosphere and can be directly conducted at room temperature, and has wide application prospect in the field of functional materials. However, LaCrO3The problems of brittleness, difficult processing and the like exist, so that large and complex products are difficult to produce, and the application of the method in the industrial field is limited to a great extent. The development of the ceramic connection technology solves the problem, ceramic products with simple shapes and easy processing can be connected together by the ceramic connection technology to prepare large samples with complex shapes, some samples which can not be processed at one time can be prepared by the ceramic connection technology, the ceramic with local damage can be repaired by the ceramic connection technology, the service life of the ceramic is prolonged, the environment is protected, the cost is saved, and the LaCrO is greatly widened3The application range of the ceramic.
LaCrO3The ceramic has the defects of low toughness, poor reliability, formability and processability and the like, so that LaCrO is caused3The application of ceramics in the industrial field is greatly limited. At present, LaCrO is used3The ceramic connection process has the defects of long time consumption, uneven element distribution in the connection area of the connecting piece, poor structural integrity of the connecting piece and the like, so that the prepared LaCrO3The ceramic connecting piece has the problems of low hardness or strength, poor compactness and the like, thereby limiting the LaCrO3Application of ceramics.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a LaCrO with short time consumption, uniform element distribution in a connection region and high structural integrity3Ceramic joining methods, i.e. with ZrB2Composite interlayer connection LaCrO3Ceramic process to solve the current LaCrO3LaCrO prepared by ceramic connection process3The ceramic connecting piece has the problems of low strength and the like.
In order to solve the technical problems, the invention provides the following technical scheme:
ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the following steps:
(1) preparation of intermediate connection layer powder: reacting ZrB2The powder and Al powder are fully mixed to obtain ZrB2-an Al mixed powder; using absolute ethyl alcohol as grinding medium to treat ZrB2Grinding the Al mixed powder for the first time, drying the Al mixed powder in a blast drier after grinding, and grinding the Al mixed powder for the second time after drying to obtain the intermediate connecting layer ZrB2-Al powder;
(2) preparing the intermediate connecting layer round sheet: to the intermediate connection layer ZrB2Adding polyvinyl alcohol solution into Al powder, grinding uniformly, drying, and pressing the mixed powder into round slices by a tablet press to obtain middle connecting layer round slices; polyvinyl alcohol solution is used as a binder to achieve the purpose of improving the cold press molding capacity of the intermediate layer powder;
(3)LaCrO3pretreatment of a ceramic base material: firstly, using sand paper to make LaCrO3Roughly polishing the ceramic base material, and then polishing the LaCrO by using a grinding and polishing machine3Polishing the surface to be connected of the ceramic base material, and polishing the LaCrO3Putting the ceramic parent material into an ethanol solution for ultrasonic cleaning, and putting the cleaned ceramic parent material into a drying oven for drying to obtain the LaCrO to be connected3A ceramic base material;
(4) spark plasma sintering connection: subjecting the LaCrO to be connected to3Assembling the ceramic parent material and the middle connecting layer round sheet into a graphite mould, putting the assembled graphite mould into a discharge plasma sintering furnace, applying pressure, keeping the whole process in a pressurized and vacuumized state, sintering, and obtaining the ZrB after sintering2Composite interlayer connection LaCrO3A ceramic connector.
The above-mentioned material is ZrB2Composite interlayer connection LaCrO3Process for the preparation of a ceramic, in step (1), ZrB2And Al in a molar ratio of 1: (0.6-1).
The above-mentioned material is ZrB2Composite interlayer connection LaCrO3Process for the preparation of a ceramic, in step (1), ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent, and the average grain diameter is 40 mu m. Tests show that the high-purity and superfine ZrB with the purity and the grain size2The powder and the Al powder are beneficial to reducing the sintering temperature and enhancing the normal-temperature bending strength of the prepared connector joint.
Above-mentioned with ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the step (1) of mixing the mass of absolute ethyl alcohol and ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 1.5-2 h, and the grinding time of the second grinding is 0.5-1 h; the drying temperature of the forced air dryer is 90 ℃, and the drying time is 10 h.
The above-mentioned material is ZrB2Composite interlayer connection LaCrO3In the step (2), the alcoholysis degree of polyvinyl alcohol is 87.0-89.0% (mol/mol), the concentration of the polyvinyl alcohol solution is 5 wt%, and the mass of the polyvinyl alcohol solution and the intermediate connecting layer ZrB2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃ and the drying time is 6 h.
The above-mentioned material is ZrB2Composite interlayer connection LaCrO3In the step (3), the volume fraction of ethanol in the ethanol solution is 95%, the ultrasonic power is 60-80 kHz, and the ultrasonic time is 30 min; the drying temperature is 50 ℃, and the drying time is 3 hours; the grinding and polishing suspension used in polishing is 0.05-9 μm diamond grinding and polishing suspension.
Above-mentioned with ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the step (4) of bonding the LaCrO3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3Sequentially assembling the ceramic base materials into a graphite mold to ensure that the center of the middle connecting layer circular sheet and the upper and lower LaCrO to be connected3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; vacuumizing the furnace to below 10Pa at room temperature; and in the sintering process, slowly applying axial pressure until the axial pressure is 30 MPa. Slowly applying pressure to discharge LaCrO to be connected3The gas in the ceramic base material and the middle connecting layer round thin sheet enables the connecting middle layer to be more compact, so that the strength of the connecting piece is higher, and meanwhile, researches show that the LaCrO can be treated when the pressure exceeds 30MPa3The connecting members are damaged to some extent and pressedThe force less than 30MPa is not favorable for LaCrO to be connected3The ceramic base material and the intermediate connection layer are connected to each other by the circular thin plate, so that the connection pressure is selected to be 30 MPa.
The above-mentioned material is ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the following steps in step (4): heating to 1300-1500 ℃ at a heating rate of 100 ℃/min, and preserving heat for 5-10 min at the temperature; and then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure, stopping vacuumizing, and finishing sintering after cooling to room temperature. During sintering, the slow temperature rise rate is not favorable for high-efficiency production of products, and the fast temperature rise rate is not favorable for full reaction of raw materials and gas discharge in the sintering process, so that the moderate temperature rise rate is selected to be 100 ℃/min; the higher sintering temperature is beneficial to the combination of the intermediate layer and the ceramic base material and improves the combination strength, but with the increase of the sintering temperature, LaCrO3The Cr in the alloy volatilizes more and more, and then not only can the LaCrO3The bonding strength of the connecting piece is reduced, and the performance of the connecting piece is also reduced, so the sintering temperature of the connecting piece is 1300-1500 ℃; the heat preservation time during sintering mainly determines the degrees of atomic diffusion and interface reaction, and researches show that the influence of the heat preservation time on the connection strength is relatively small, so that the proper heat preservation time is selected for 5-10 min.
The above-mentioned material is ZrB2The composite intermediate layer is connected with LaCrO3Process for producing ceramics, said LaCrO3The ceramic base material is a cylinder, and the LaCrO3The diameter of the ceramic base material is equal to that of the middle connecting layer round sheet.
The above-mentioned material is ZrB2Composite interlayer connection LaCrO3Process for the preparation of a ceramic, in step (1), ZrB2And Al in a molar ratio of 1: (0.6 to 1); ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent, and the average grain diameter is 40 mu m; mass of absolute ethanol and said ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 1.5-2 h, and the grinding time of the second grinding is 0.5-1 h; the drying temperature of the blast drier is 90 ℃, and the drying time is 10 hours;
in the step (2), the alcoholysis degree of the polyvinyl alcohol is 87.0-89.0% (mol/mol), the concentration of the polyvinyl alcohol solution is 5 wt%, and the mass of the polyvinyl alcohol solution and the intermediate connecting layer ZrB2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃, and the drying time is 6 hours;
in the step (3), the volume fraction of ethanol in the ethanol solution is 95%, the ultrasonic power is 60-80 kHz, and the ultrasonic time is 30 min; the drying temperature is 50 ℃, and the drying time is 3 hours; the grinding and polishing suspension used in polishing is 0.05-9 mu m diamond grinding and polishing suspension;
in the step (4), LaCrO is connected according to the ratio3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3Sequentially assembling the ceramic base materials into a graphite mold to ensure that the center of the middle connecting layer circular sheet and the upper and lower LaCrO to be connected3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; vacuumizing the furnace at room temperature until the vacuum degree is less than or equal to 10Pa, and slowly applying axial pressure until the axial pressure is 30MPa in the sintering process;
in the step (4), the sintering process is as follows: heating to 1300-1500 ℃ at a heating rate of 100 ℃/min, and preserving heat for 5-10 min at the temperature; then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure and stopping vacuumizing, and finishing sintering after cooling to room temperature;
the LaCrO3The ceramic base material is a cylinder, and the LaCrO3The diameter of the ceramic base material is equal to that of the middle connecting layer round sheet.
The technical principle of the invention is as follows:
with the development of connection technology, the connecting piece is made of various materials, sometimes a single intermediate layer cannot meet the connection requirement, and in order to obtain a joint which meets the connection requirement and is more stable and reliable, researchers compound different intermediate layer materials to obtain a compound intermediate layer meeting the connection condition. ZrB2Has the same LaCrO3Ceramics have many similar excellent properties: high melting point and hardnessHigh elastic modulus, good heat conductivity, good electrical conductivity and the like. Albeit ZrB2Coefficient of thermal expansion and LaCrO3The ceramics have some differences, but the conductivity far exceeds that of LaCrO3The ceramic can be used for compounding ZrB with other materials under the condition of meeting the conductive performance of the connecting piece2Is optimally adjusted.
To ZrB2The addition of metal powder into the composite ceramic material can raise the heat expansion coefficient of ceramic product, so that it can add metal powder into ZrB2Adding Al powder into the powder to prepare ZrB2-an Al composite material. Due to ZrB2Coefficient of thermal expansion and LaCrO3The mismatching of ceramics can cause the residual stress of the connecting piece to be larger during high-temperature connection, and the ZrB can be obtained at lower temperature after Al powder is added2The sintering provides a liquid environment, reduces the sintering temperature, promotes the densification of the material at a lower temperature, and is also beneficial to improving ZrB2And reduces residual thermal stress at the joint. Thus, by preparing ZrB2-Al composite material as a joint LaCrO3An intermediate layer of ceramic.
The technical scheme of the invention achieves the following beneficial technical effects:
(1) the invention controls ZrB2The ratio of Al powder to Al powder and related preparation process parameters, for LaCrO3Carrying out spark plasma sintering connection on the ceramics; ZrB is obtained by the in-situ reaction of mixed powder at relatively low temperature and short holding time2The LaCrO is realized at the same time of the-Al composite ceramic connecting layer3And (5) connecting the ceramics. In one aspect, ZrB2Is compounded with Al to ensure that the thermal expansion coefficient of the connecting interlayer is more matched with that of the lanthanum chromate ceramic, thereby reducing the connecting interlayer and the LaCrO3The residual stress between the ceramic base materials realizes good interface connection, avoids the formation of joint cracks and improves the strength of the joint. ZrB on the other hand2The electrical resistivity of the-Al composite ceramic connecting layer is far lower than that of the mother material to be connected LaCrO3The resistivity of the connecting piece can completely meet the conductive performance requirement of the connecting piece in the conductive performance.
(2) The LaCrO prepared by the preparation process of the invention3The joint of the ceramic connecting piece has the bending strength of 23.79MPa at the maximum at normal temperature; the highest Vickers hardness of the middle connecting layer is 7.01GPa, the density is 89.06-99.29%, and the resistivity is 0.03-0.04 m omega/cm3. The skilled artisan also finds that during sintering, when the temperature rise rate is greater than 100 ℃/min or less than 100 ℃/min, or the temperature fall rate is greater than 50 ℃/min or less than 50 ℃/min, the ZrB can be adjusted in any way2The molar ratio of Al to the raw material, the sintering temperature and the heat preservation time, and the prepared LaCrO3The hardness, the normal-temperature bending strength and the compactness of the ceramic connecting piece cannot achieve the effect when the heating rate is 100 ℃/min or the cooling rate is 50 ℃/min, which is probably because when the heating rate is 100 ℃/min and the cooling rate is 50 ℃/min, the elements in the connecting area can be more uniformly distributed.
Drawings
FIG. 1 LaCrO in the invention3The connection structure of the ceramic connecting piece is shown schematically;
FIG. 2 shows LaCrO obtained by sintering intermediate connection layer powder of different raw material ratios at different temperatures3Normal temperature bending strength of the ceramic connecting piece;
FIG. 3 LaCrO prepared in example 1 of the present invention3Cross-sectional SEM images of ceramic connectors;
FIG. 4 LaCrO prepared in example 2 of the present invention3Cross-sectional SEM images of ceramic connectors;
FIG. 5 LaCrO prepared in example 3 of the present invention3Cross-sectional SEM image of ceramic connector.
Detailed Description
Example 1
ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the following steps:
(1) preparation of intermediate connection layer powder: reacting ZrB2The powder and Al powder are fully mixed to obtain ZrB2-an Al mixed powder; reacting ZrB2Putting the-Al mixed powder into agate grinding, taking absolute ethyl alcohol as a grinding medium, grinding for the first time, and performing grindingAnd then putting the intermediate connection layer ZrB into a blast drier for drying, and grinding for the second time after drying is finished to obtain the intermediate connection layer ZrB2-Al powder;
(2) preparing the intermediate connecting layer round sheet: to the intermediate connection layer ZrB2Adding polyvinyl alcohol solution into Al powder, grinding uniformly, drying, and pressing the mixed powder into round slices by a tablet press to obtain middle connecting layer round slices;
(3)LaCrO3pretreatment of a ceramic base material: firstly, using sand paper to make LaCrO3Roughly polishing the ceramic base material, and then polishing the LaCrO by using a grinding and polishing machine3Polishing the surface to be connected of the ceramic base material, and polishing the LaCrO3Putting the ceramic parent material into an ethanol solution for ultrasonic cleaning, and putting the cleaned ceramic parent material into a drying oven for drying to obtain the LaCrO to be connected3A ceramic base material;
(4) spark plasma sintering connection: subjecting the LaCrO to be connected to3Assembling the ceramic parent metal and the intermediate connection layer round sheet into a graphite mold, then putting the assembled graphite mold into a discharge plasma sintering furnace, applying pressure, keeping the whole process in a pressurized and vacuumized state, sintering, and obtaining ZrB after sintering2Composite interlayer connection LaCrO3A ceramic connector.
In step (1), ZrB2And Al in a molar ratio of 1: 0.8; ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent, and the average grain diameter is 40 mu m; mass of absolute ethanol and said ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 2 hours, and the grinding time of the second grinding is 1 hour; the drying temperature of the forced air dryer is 90 ℃, and the drying time is 10 h.
In the step (2), the alcoholysis degree of the polyvinyl alcohol is 87.0 percent (mol/mol), the concentration of the polyvinyl alcohol solution is 5 weight percent, and the mass of the polyvinyl alcohol solution and the mass of the intermediate connecting layer ZrB2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃, and the drying time is 6 hours; the diameter of the middle connecting layer round sheet is 18 mm.
In the step (3), ethanol is dissolvedThe volume fraction of ethanol in the liquid is 95%, the ultrasonic power is 60kHz, and the ultrasonic cleaning time is 30 min; the drying temperature is 50 ℃ and the drying time is 3 h. The grinding and polishing suspension used in polishing is 0.05-9 mu m diamond grinding and polishing suspension; the LaCrO3The ceramic base material is a cylinder with the diameter of 18 mm.
In the step (4), LaCrO is connected according to the ratio3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3The ceramic base materials are sequentially assembled into a graphite mold (see figure 1), and the centers of the middle connecting layer round sheets and the upper and lower LaCrO to be connected are ensured3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; vacuumizing the furnace to below 10Pa at room temperature; and in the sintering process, slowly applying axial pressure until the axial pressure is 30 MPa.
The sintering process is as follows: heating to 1300 deg.C at a heating rate of 100 deg.C/min, and maintaining at the temperature for 5 min; and then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure, stopping vacuumizing, and finishing sintering after cooling to room temperature.
Through detection, LaCrO prepared in the embodiment3The normal-temperature bending strength of the joint of the ceramic connecting piece is 13.26MPa, the thickness of the middle connecting layer is 100 mu m, the Vickers hardness of the middle connecting layer is 3.44GPa, the density is 89.06 percent, and the resistivity is 0.04m omega/cm3。
Example 2
ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the following steps:
(1) preparation of intermediate connection layer powder: reacting ZrB2The powder and Al powder are fully mixed to obtain ZrB2-an Al mixed powder; reacting ZrB2Putting the Al mixed powder into agate grinding, taking absolute ethyl alcohol as a grinding medium, grinding for the first time, putting the mixture into a blast drier for drying after grinding, and grinding for the second time after drying to obtain the intermediate connecting layer ZrB2-Al powder;
(2) preparing the intermediate connecting layer round sheet: to the intermediate connection layer ZrB2Adding polyvinyl alcohol solution into Al powder, grinding uniformly, drying, and pressing the mixed powder into round slices by a tablet press to obtain middle connecting layer round slices;
(3)LaCrO3pretreatment of a ceramic base material: firstly, using sand paper to make LaCrO3Roughly polishing the ceramic base material, and then polishing the LaCrO by using a grinding and polishing machine3Polishing the surface to be connected of the ceramic base material, and polishing the LaCrO3Putting the ceramic parent material into an ethanol solution for ultrasonic cleaning, and putting the cleaned ceramic parent material into a drying oven for drying to obtain the LaCrO to be connected3A ceramic base material;
(4) spark plasma sintering connection: subjecting the LaCrO to be connected to3Assembling the ceramic parent metal and the intermediate connection layer round sheet into a graphite mold, then putting the assembled graphite mold into a discharge plasma sintering furnace, applying pressure, keeping the whole process in a pressurized and vacuumized state, sintering, and obtaining ZrB after sintering2Composite interlayer connection LaCrO3A ceramic connector.
In step (1), ZrB2And Al in a molar ratio of 1: 1; ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent, and the average grain diameter is 40 mu m; mass of absolute ethanol and said ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 2 hours, and the grinding time of the second grinding is 1 hour; the drying temperature of the forced air dryer is 90 ℃, and the drying time is 10 h.
In the step (2), the alcoholysis degree of the polyvinyl alcohol is 88.0 percent (mol/mol), the concentration of the polyvinyl alcohol solution is 5 weight percent, and the mass of the polyvinyl alcohol solution and the intermediate connecting layer ZrB2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃, and the drying time is 6 hours; the diameter of the middle connecting layer round sheet is 15 mm.
In the step (3), the volume fraction of ethanol in the ethanol solution is 95%, the ultrasonic power is 60kHz, and the ultrasonic cleaning time is 30 min; the drying temperature is 50 ℃ and the drying time is 3 h. The grinding and polishing suspension used in polishing is 0.05-9 mu m diamond grinding and polishing suspension; the LaCrO3The ceramic base material is a cylinder with the diameter of 15 mm.
In the step (4), LaCrO is connected according to the ratio3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3Sequentially assembling the ceramic base materials into a graphite mold to ensure that the center of the middle connecting layer circular sheet and the upper and lower LaCrO to be connected3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; vacuumizing the furnace to below 10Pa at room temperature; and in the sintering process, slowly applying axial pressure until the axial pressure is 30 MPa.
The sintering process comprises the following steps: heating to 1400 deg.C at a heating rate of 100 deg.C/min, and maintaining at the temperature for 5 min; and then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure, stopping vacuumizing, and finishing sintering after cooling to room temperature.
Through detection, LaCrO prepared in the embodiment3The normal-temperature bending strength of the joint of the ceramic connecting piece is 20.43MPa, the thickness of the middle connecting layer is 90 mu m, the Vickers hardness of the middle connecting layer is 5.24GPa, the density is 94.14 percent, and the resistivity is 0.03m omega/cm3。
Example 3
ZrB2Composite interlayer connection LaCrO3The ceramic process comprises the following steps:
(1) preparation of intermediate connection layer powder: reacting ZrB2The powder and Al powder are fully mixed to obtain ZrB2-an Al mixed powder; reacting ZrB2Putting the Al mixed powder into agate grinding, taking absolute ethyl alcohol as a grinding medium, grinding for the first time, putting the mixture into a blast drier for drying after grinding, and grinding for the second time after drying to obtain the intermediate connecting layer ZrB2-Al powder;
(2) preparing the intermediate connecting layer round sheet: to the intermediate connection layer ZrB2Adding polyvinyl alcohol solution into Al powder, grinding uniformly, drying, and pressing the mixed powder into round slices by a tablet press to obtain middle connecting layer round slices;
(3)LaCrO3pretreatment of a ceramic base material: firstly, using sand paper to make LaCrO3Ceramic materialRough grinding is carried out on the base material, and then the LaCrO is ground by a grinding and polishing machine3Polishing the surface to be connected of the ceramic base material, and polishing the LaCrO3Putting the ceramic parent material into an ethanol solution for ultrasonic cleaning, and putting the cleaned ceramic parent material into a drying oven for drying to obtain the LaCrO to be connected3A ceramic base material;
(4) spark plasma sintering connection: subjecting the LaCrO to be connected to3Assembling the ceramic parent metal and the intermediate connection layer round sheet into a graphite mold, then putting the assembled graphite mold into a discharge plasma sintering furnace, applying pressure, keeping the whole process in a pressurized and vacuumized state, sintering, and obtaining ZrB after sintering2Composite interlayer connection LaCrO3A ceramic connector.
In step (1), ZrB2And Al in a molar ratio of 1: 1; ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent, and the average grain diameter is 40 mu m; mass of absolute ethanol and said ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 2 hours, and the grinding time of the second grinding is 1 hour; the drying temperature of the forced air dryer is 90 ℃, and the drying time is 10 h.
In the step (2), the alcoholysis degree of the polyvinyl alcohol is 89.0 percent (mol/mol), the concentration of the polyvinyl alcohol solution is 5 weight percent, and the mass of the polyvinyl alcohol solution and the intermediate connecting layer ZrB2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃, and the drying time is 6 hours; the diameter of the middle connecting layer round sheet is 25 mm.
In the step (3), the volume fraction of ethanol in the ethanol solution is 95%, the ultrasonic power is 60kHz, and the ultrasonic cleaning time is 30 min; the drying temperature is 50 ℃ and the drying time is 3 h. The grinding and polishing suspension used during polishing is 0.05-9 mu m diamond grinding and polishing suspension; the LaCrO3The ceramic base material is a cylinder with the diameter of 25 mm.
In the step (4), LaCrO is connected according to the ratio3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3The sequential assembly of the ceramic parent material into the graphite mold, ensuring the sameThe center of the middle connecting layer circular sheet and the upper and lower LaCrO to be connected3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; vacuumizing the furnace to below 10Pa at room temperature; and in the sintering process, slowly applying axial pressure until the axial pressure is 30 MPa.
The sintering process is as follows: heating to 1500 ℃ at a heating rate of 100 ℃/min, and keeping the temperature for 10 min; and then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure, stopping vacuumizing, and finishing sintering after cooling to room temperature.
Through detection, LaCrO prepared in the embodiment3The normal-temperature bending strength of the joint of the ceramic connecting piece is 23.79MPa, the thickness of the middle connecting layer is 95 mu m, the Vickers hardness of the middle connecting layer is 7.01GPa, the density is 99.29 percent, and the resistivity is 0.03m omega/cm3。
FIGS. 3 to 5 are SEM images of the connecting members prepared in examples 1 to 3, respectively, and it can be seen from comparison of FIGS. 3 to 5 that the intermediate connecting layer has reduced pores and increased density with increased temperature, wherein the intermediate connecting layer and LaCrO of the connecting member of FIG. 53The interface of the ceramic base material becomes unclear, which shows that the intermediate connection layer and the LaCrO3The ceramic base material has good interface connection effect, and the connection of the connection part is tight.
In summary, the invention passes ZrB at a relatively low temperature and short holding time2ZrB is obtained by the in-situ reaction of the mixed powder with Al2The Al-composite ceramic connecting layer simultaneously realizes LaCrO3And (5) connecting the ceramics. The composite ceramic connecting layer has a structure similar to that of LaCrO3The ceramics parent material has similar thermophysical properties, the thermal expansion coefficients of the ceramics parent material and the ceramics parent material are similar, the ceramics parent material has good interface connection effect, and the resistivity is far lower than that of LaCrO3Ceramic, without affecting its electrical conductivity. With ZrB2The intermediate layer was a mixed powder of Al 1:1 (molar ratio), and a joining temperature of 1500 ℃ gave a joining material having a high room-temperature bending strength. The invention can prepare high-strength LaCrO3Ceramic connecting piece, solve the problem of LaCrO3The problem of difficult processing in ceramic engineering application can be solved simultaneouslyThe technology repairs the locally damaged ceramics, prolongs the service life of the ceramics, protects the environment, saves the cost and greatly widens the LaCrO3The application range of the ceramic.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are possible which remain within the scope of the appended claims.
Claims (10)
1. ZrB2Composite interlayer connection LaCrO3The ceramic process is characterized by comprising the following steps:
(1) preparation of intermediate connection layer powder: reacting ZrB2The powder and Al powder are fully mixed to obtain ZrB2-an Al mixed powder; using absolute ethyl alcohol as grinding medium to treat ZrB2Grinding the Al mixed powder for the first time, drying the Al mixed powder in a blast drier after grinding, and grinding the Al mixed powder for the second time after drying to obtain the intermediate connecting layer ZrB2-Al powder;
(2) preparing the intermediate connecting layer round sheet: to the intermediate connection layer ZrB2Adding polyvinyl alcohol solution into Al powder, grinding uniformly, drying, and pressing the mixed powder into round slices by a tablet press to obtain middle connecting layer round slices;
(3)LaCrO3pretreatment of a ceramic base material: firstly, using sand paper to make LaCrO3Roughly polishing the ceramic base material, and then polishing the LaCrO by using a grinding and polishing machine3Polishing the surface to be connected of the ceramic base material, and polishing the LaCrO3Putting the ceramic parent material into an ethanol solution for ultrasonic cleaning, and putting the cleaned ceramic parent material into a drying oven for drying to obtain the LaCrO to be connected3A ceramic base material;
(4) spark plasma sintering connection: subjecting the LaCrO to be connected to3Assembling the ceramic base material and the intermediate connection layer round thin sheet into a graphite mold, and assemblingPutting the graphite mold into a discharge plasma sintering furnace, applying pressure, keeping the whole process in a pressurized and vacuumized state, sintering, and obtaining ZrB after sintering2Composite interlayer connection LaCrO3A ceramic connector.
2. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3Process for ceramics, characterized in that in step (1), ZrB2And Al in a molar ratio of 1: (0.6-1).
3. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3Process for ceramics, characterized in that in step (1), ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent, and the average grain diameter is 40 mu m.
4. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3The process of the ceramic is characterized in that in the step (1), the mass of the absolute ethyl alcohol and the ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 1.5-2 h, and the grinding time of the second grinding is 0.5-1 h; the drying temperature of the forced air dryer is 90 ℃, and the drying time is 10 h.
5. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3The ceramic process is characterized in that in the step (2), the alcoholysis degree of polyvinyl alcohol is 87.0-89.0% (mol/mol), the concentration of the polyvinyl alcohol solution is 5 wt%, and the mass of the polyvinyl alcohol solution and the intermediate connecting layer ZrB are2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃ and the drying time is 6 h.
6. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3The ceramic process is characterized in that in the step (3), the volume fraction of ethanol in the ethanol solution is 95 percent and is overThe sound power is 60-80 kHz, and the ultrasonic time is 30 min; the drying temperature is 50 ℃, and the drying time is 3 hours; the grinding and polishing suspension used in polishing is 0.05-9 μm diamond grinding and polishing suspension.
7. The stabilized ZrB of claim 12The composite intermediate layer is connected with LaCrO3The ceramic process is characterized in that in the step (4), LaCrO is connected according to the ratio3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3Sequentially assembling the ceramic base materials into a graphite mold to ensure that the center of the middle connecting layer circular sheet and the upper and lower LaCrO to be connected3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; and (3) vacuumizing the furnace at room temperature until the vacuum degree is less than or equal to 10Pa, and slowly applying axial pressure until the axial pressure is 30MPa in the sintering process.
8. The catalyst of claim 1 with ZrB2The composite intermediate layer is connected with LaCrO3The ceramic process is characterized in that in the step (4), the sintering process is as follows: heating to 1300-1500 ℃ at a heating rate of 100 ℃/min, and preserving heat for 5-10 min at the temperature; and then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure, stopping vacuumizing, and finishing sintering after cooling to room temperature.
9. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3The process of the ceramic is characterized in that the LaCrO is3The ceramic base material is a cylinder, and the LaCrO3The diameter of the ceramic base material is equal to that of the middle connecting layer round sheet.
10. The catalyst of claim 1 with ZrB2Composite interlayer connection LaCrO3Process for ceramics, characterized in that in step (1), ZrB2And Al in a molar ratio of 1: (0.6 to 1); ZrB2The purity of the powder is more than 99 percent, and the average grain diameter is 1 mu m; the purity of the Al powder is more than 99 percent,and the average particle diameter is 40 μm; mass of absolute ethanol and said ZrB2The mass ratio of the Al mixed powder is 1.2:1, the grinding time of the first grinding is 1.5-2 h, and the grinding time of the second grinding is 0.5-1 h; the drying temperature of the forced air drier is 90 ℃, and the drying time is 10 h;
in the step (2), the alcoholysis degree of the polyvinyl alcohol is 87.0-89.0% (mol/mol), the concentration of the polyvinyl alcohol solution is 5 wt%, and the mass of the polyvinyl alcohol solution and the intermediate connecting layer ZrB2-the mass ratio of Al powder is 4: 10; the drying temperature is 90 ℃, and the drying time is 6 hours;
in the step (3), the volume fraction of ethanol in the ethanol solution is 95%, the ultrasonic power is 60-80 kHz, and the ultrasonic time is 30 min; the drying temperature is 50 ℃, and the drying time is 3 hours; the grinding and polishing suspension used in polishing is 0.05-9 mu m diamond grinding and polishing suspension;
in the step (4), LaCrO is connected according to the ratio3Ceramic base material, the intermediate connection layer round sheet and the LaCrO to be connected3Sequentially assembling ceramic base materials into a graphite mold to ensure the center of the middle connecting layer circular sheet and the upper and lower LaCrO to be connected3The centers of the connecting surfaces of the ceramic base materials are positioned on the same straight line; vacuumizing the furnace at room temperature until the vacuum degree is less than or equal to 10Pa, and slowly applying axial pressure until the axial pressure is 30MPa in the sintering process;
in the step (4), the sintering process is as follows: heating to 1300-1500 ℃ at a heating rate of 100 ℃/min, and preserving heat for 5-10 min at the temperature; then cooling to 100 ℃ at a cooling rate of 50 ℃/min, stopping heating, stopping applying pressure and stopping vacuumizing, and finishing sintering after cooling to room temperature;
the LaCrO3The ceramic base material is a cylinder, and the LaCrO3The diameter of the ceramic base material is equal to that of the middle connecting layer circular sheet.
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Application publication date: 20211029 Assignee: Dongfang Runpeng Technology (Beijing) Group Co.,Ltd. Assignor: INNER MONGOLIA University OF TECHNOLOGY Contract record no.: X2024980009219 Denomination of invention: A process of connecting LaCrO3ceramics with ZrB2composite intermediate layer Granted publication date: 20220610 License type: Common License Record date: 20240709 |