CN101575216B - SPS connecting method of the same material or different materials between SiAlON ceramic and Si3N4 ceramic - Google Patents
SPS connecting method of the same material or different materials between SiAlON ceramic and Si3N4 ceramic Download PDFInfo
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- CN101575216B CN101575216B CN2009100722933A CN200910072293A CN101575216B CN 101575216 B CN101575216 B CN 101575216B CN 2009100722933 A CN2009100722933 A CN 2009100722933A CN 200910072293 A CN200910072293 A CN 200910072293A CN 101575216 B CN101575216 B CN 101575216B
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Abstract
The present invention relates to an SPS connecting method of the same material or different materials between SiAlON ceramic and Si3N4 ceramic, which pertains to the ceramic material connection field. The invention solves the problems of complicated technique conditions, low working efficiency, high energy consumption and low joint strength during the connection of ceramic materials. The method comprises the following steps: 1. leveling the surface of the base metal to be welded and washing the surface with ethanol, and 2. connecting with the SPS method. The SPS connecting method provided by the present invention has the advantages of simple technique, high working efficiency, low energy consumption and high joint strength which is more powerful than that of the base metal.
Description
Technical field
The invention belongs to the connection area of stupalith, relate to a kind of SiAlON pottery, Si
3N
4Pottery SPS method of attachment of the same race or xenogeneic.
Background technology
SiAlON and Si
3N
4Pottery has excellent mechanical property and corrosion-resistant, wear-resistant ability, is use one of high temperature resistant structure ceramics and cutter material widely.
In breakage reparation and machinofacture process, often need link together ceramic member.Disclosed method of attachment has three kinds.First method is soldering.But because SiAlON or Si
3N
4Pottery is difficult to wetted, connects so must adopt special active solder just can finish soldering.Active solder commonly used is to add Ag-Cu alloy [the 228th page of Materials science and technology the 13rd 3 phase of volume of June in 2005 of containing 10% Ti, V, Zr, Hf, Nb or Ta isoreactivity element, patent No. ZL 200710087292.7, patent No. ZL 200410043962.1, number of patent application 200610010356.9].
Another kind method is with Si
3N
4The intergranular of pottery coordinates and is divided into scolder, carries out reaction soldering [the 130th page of ceramic journal the 23rd 2 phase of volume of June in 2002].Solder compositions is with Y
2O
3-Al
2O
3-SiO
2, La
2O
3-Al
2O
3-SiO
2(La is a lanthanon) or MgO-Al
2O
3-SiO
2Oxide compound is the basis, adds a spot of α-Si
3N
4, can utilize the β-Si of generation
3N
4Improve strength of joint; Change the type or the content of oxide compound, can improve the heat resisting temperature of joint.The reaction soldering connection method needs certain pressure, and auxiliary scolder is being connected surface spreading, forms fine and close joint.The Si that 5MPa/1600 ℃/30min connects
3N
4Pottery, strength of joint can reach 80% of strength of parent, but maximum operation (service) temperature is no more than 1200 ℃.
Cause strength of joint to be lower than mother metal and the not high reason of joint use temperature has three: the one, joint itself is the low strength phase, its mechanical property is not high; The second, scolder is different with the thermal expansivity of mother metal, causes that very big thermal stresses is arranged in the joint; The 3rd, the non-refractory of scolder own.For improving the room temperature and the mechanical behavior under high temperature of joint, need adopt more infusible solder flux usually; Reduce the coefficient of thermal expansion mismatch of joint and mother metal; Eliminate the macroscopic interface of weld seam by abundant diffusion.
Si
3N
4The third method of attachment of pottery is pressure diffusion welding, uses conventional hot pressed sintering equipment, and the composition under the dependence high-temperature pressurizing condition spreads realizes Si
3N
4The connection of pottery.Generally need make Si soak more than 1600 ℃ several hours
3N
4Crystal grain is grown in seam, remedies the highly malleablized mechanism of joint.Be elimination seam and the weave construction of mother metal and the difference of performance, even the high welding pressure of employing 3GPa is to Si
3N
4Pottery connects.The High Temperature High Pressure welding has increased production cost for a long time, is difficult to application aborning.
In sum, though Si
3N
4The interconnection technique of pottery has had very big progress (report that does not still have SiAlON pottery connection aspect at present), but still have many technical barriers, mainly show as: the processing condition complexity, efficient is low, energy consumption is big, strength of joint not high (being significantly less than strength of parent).
Summary of the invention
The objective of the invention is to connect and to have processing condition complexity, inefficiency, energy consumption is big, strength of joint is low problem in order to solve stupalith; And SiAlON pottery, Si are provided
3N
4The SPS method of attachment of same material or foreign material between pottery.
SiAlON pottery, Si among the present invention
3N
4The SPS method of attachment of same material or foreign material is undertaken by following step between pottery: one, mother metal to be welded surface is polished with emery wheel whole, with ethanol flush away surface contamination and foreign material; Two, the mother metal to be welded that will handle through step 1 is connected in the face of putting, the mould of packing into is placed in SPS (plasma discharging hot pressed sintering) stove, to be evacuated down to pressure<6Pa in the SPS stove, charging into nitrogen pressure to the SPS stove again is 0.1~5MPa, increase the weldment end force when heating up then gradually, temperature rises to 700 ℃ of weldment end forces and reaches 1~100MPa, be heated to 1300~1900 ℃ with 5~200 ℃/min temperature rise rate in the time of pressurize, be incubated 0~90min again, stop heating, remove pressure, naturally cool to room temperature with stove again; SiAlON pottery, Si have promptly been finished
3N
4Pottery SPS of the same race or xenogeneic connects; Wherein the described mother metal to be welded of step 1 is SiAlON pottery, Si
3N
4Same material or foreign material between pottery.
The present invention also can be after step 2 naturally cools to room temperature with stove, weldment after connecting is carried out high-temperature heat treatment, concrete steps are as follows with parameter: the weldment after will being connected places High Temperature Furnaces Heating Apparatus again, pressure<10Pa will be evacuated down to then in the High Temperature Furnaces Heating Apparatus, charging into nitrogen pressure to the SPS stove again is 0.1~0.5MPa, be heated to 1300~1900 ℃ with 5~100 ℃/min temperature rise rate then, high-temperature heat treatment 30~1800min under 1300~1900 ℃ of conditions, stop heating then, naturally cool to room temperature with stove again, promptly finished thermal treatment the weldment after connecting.
The present invention has following advantage:
(1) the inventive method has high efficiency, technology is simple, energy consumption is little advantage, and the present invention adopts the SPS method, and (but also time expand by several hours) can realize SiAlON pottery and Si in tens minutes
3N
4Of the same race or xenogenesis between the pottery connects, thereby has improved working efficiency, reduced energy consumption; (2) strength of joint is greater than strength of parent; (3) do not use solder, the macroscopic view of the jointing of same material, micro components and tissue and mother metal are just the same, and no thermal mismatch stress has fundamentally been eliminated the influence of joint to strength of joint; Optimize SiAlON or Si when (4) can realize the structure properties of mother metal, joint by follow-up high-temperature heat treatment
3N
4Crystal grain strides across the weld seam growth, can further eliminate the difference of the weave construction of joint and mother metal, improves welding quality.
Description of drawings
Fig. 1 is SiAlON and Si
3N
4Workpiece dress mould synoptic diagram in the stupalith SPS method of attachment, 1 expression pressure head among Fig. 1,2 expression moulds, 3 expressions mother metal to be welded, P representative pressure; Photo in kind after Fig. 2 embodiment 14 connects; Fig. 3 is the low power shape appearance figure of 1700 ℃/20MPa/0min processing condition lower sub in the embodiment 15; The high power shape appearance figure of 1700 ℃/20MPa/10min processing condition lower sub in Fig. 4 embodiment 15; Fig. 5 is the strength of joint of embodiment 15 and the graph of a relation of weld interval, among Fig. 5-the strength of joint curve of-expression embodiment 15 described weld seams, the intensity of α-SiAlON ceramic welding mother metal of zero expression doped metal ion Yb, △ represents the intensity of α-SiAlON ceramic welding mother metal of doped metal ion Y; Fig. 6 is the low power shape appearance figure of the joint after embodiment 16 thermal treatments; Fig. 7 is the high power shape appearance figure of the joint after embodiment 16 thermal treatments.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: SiAlON pottery, Si in the present embodiment
3N
4Pottery SPS method of attachment of the same race or xenogeneic is undertaken by following step: one, mother metal to be welded surface is polished with emery wheel whole, with ethanol flush away surface contamination and foreign material; Two, the mother metal to be welded that will handle through step 1 is connected in the face of putting, the mould of packing into is placed in SPS (plasma discharging hot pressed sintering) stove, to be evacuated down to pressure<6Pa in the SPS stove, charging into nitrogen pressure to the SPS stove again is 0.1~5MPa, increase the weldment end force when heating up then gradually, temperature rises to 700 ℃ of weldment end forces and reaches 1~100MPa, be heated to 1300~1900 ℃ with 5~200 ℃/min temperature rise rate in the time of pressurize, be incubated 0~90min again, stop heating, remove pressure, naturally cool to room temperature with stove again; SiAlON pottery, Si have promptly been finished
3N
4Pottery SPS of the same race or xenogeneic connects; Wherein the described mother metal to be welded of step 1 is SiAlON pottery, Si
3N
4Same material or foreign material between pottery.
Present embodiment adopts SPS (discharge plasma sintering) method to realize SiAlON pottery, Si
3N
4The connection of same material or foreign material between pottery, strength of joint is greater than strength of parent.
Embodiment two: what present embodiment and embodiment one were different is: the weldment end force is 5~80MPa pressure in the step 2.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the weldment end force is 10~50MPa pressure in the step 2.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: the weldment end force is a 20MPa pressure in the step 2.Other step and parameter are identical with embodiment one.
Embodiment five: what present embodiment and embodiment one, two, three or four were different is: be incubated 5~20min in the step 2 under 1400~1800 ℃ of conditions.Other step and parameter are identical with embodiment one, two, three or four.
Embodiment six: what present embodiment and embodiment one, two, three or four were different is: be incubated 10min in the step 2 under 1700 ℃ of conditions.Other step and parameter are identical with embodiment one, two, three or four.
Embodiment seven: what present embodiment and embodiment one to six were different is: the described temperature rise rate of step 2 is 50~150 ℃/min.Other step and parameter are identical with embodiment one to six.
Embodiment eight: what present embodiment and embodiment one to six were different is: the described temperature rise rate of step 2 is 100 ℃/min.Other step and parameter are identical with embodiment one to six.
Embodiment nine: what present embodiment and embodiment one to eight were different is: after step 2 naturally cools to room temperature with stove, again weldment is placed High Temperature Furnaces Heating Apparatus, pressure<10Pa will be evacuated down to then in the High Temperature Furnaces Heating Apparatus, charging into nitrogen pressure to the stove again is 0.1~0.5MPa, be heated to 1300~1900 ℃ with 5~100 ℃/min temperature rise rate then, high-temperature heat treatment 30~1800min under 1300~1900 ℃ of conditions stops heating then, naturally cools to room temperature with stove again.Other step and parameter are identical with embodiment one to eight.
Embodiment ten: present embodiment is implemented nine and different is with concrete: the temperature of high-temperature heat treatment is 1500~1800 ℃.Other step and parameter are identical with embodiment one to eight.
Embodiment 11: present embodiment is implemented nine and different is with concrete: the temperature of high-temperature heat treatment is 1700 ℃.Other step and parameter are identical with embodiment nine.
Embodiment 12: present embodiment is implemented nine, ten or 11 and different is with concrete: the time of high-temperature heat treatment is 60~200min.Other step and parameter are identical with embodiment nine, ten or 11.
Embodiment 13: present embodiment is implemented nine, ten or 11 and different is with concrete: the time of high-temperature heat treatment is 120min.Other step and parameter are identical with embodiment nine, ten or 11.
Embodiment 14: the present embodiment welding base metal is that diameter is α-SiAlON pottery that 20mm, thickness are respectively 5mm and 4mm, and both design mix are Y
1/3Si
10Al
2ON
5, added the BaAl of 10% (weight), 5% (weight) respectively
2Si
2O
3As sintering agent, all be that pressureless sintering 60min makes under 1900 ℃ of conditions, in the nitrogen atmosphere of 0.5MPa, its thing constitutes mutually and is α-SiAlON, a small amount of β-SiAlON (mass percent is less than 5%) and intergranular phase BaAl
2Si
2O
3, both three-point bending strengths all are not less than 680MPa, fracture toughness property is not less than 7.8MPam
1/2Above two kinds of materials are connected, and method of attachment is the SPS method, and the concrete steps of connection are as follows: one, mother metal to be welded surface is polished with the diamond wheel of 120 order granularities whole, usefulness ethanol flush away surface contamination and foreign material; Two, the mother metal to be welded that will handle through step 1 is connected in the face of putting, the mould (as shown in Figure 1) of packing into then is placed in the SPS stove, to be evacuated down to pressure<6Pa in the SPS stove then, charging into nitrogen pressure to the SPS stove again is 0.5MPa, is warming up to 700 ℃ and weldment applied 20MPa pressure at 1~4min then, is heated to 1700 ℃ with 100 ℃/min temperature rise rate again, insulation 10min, stop heating then, remove pressure, naturally cool to room temperature with stove; The SPS that has promptly finished SiAlON pottery of the same race connects.
The model of SPS stove is SPS-2050, and manufacturer is a Japanese Sumito company.
Weldment after connecting in the 5min in the present embodiment can cool to below 800 ℃; The photo in kind of the weldment after the connection as shown in Figure 2.
The strength of joint of the weldment after after tested, present embodiment obtains to connect is than the high 20MPa of strength of parent.
Embodiment 15: the present embodiment welding base metal is that diameter is 20mm, thickness and is 7mm, α-SiAlON pottery of doped metal ion Y and Yb respectively, and chemical formula is respectively Y
0.4Si
9.6Al
2.4O
1.2N
14.8And Yb
0.4Si
9.6Al
2.4O
1.2N
14.8, all be to adopt the SPS sintering process in the nitrogen atmosphere of 0.1MPa, to apply sintering 10min synthetic under 20MPa pressure, the 1750 ℃ of conditions; Its thing constitutes mutually and is α-SiAlON, a small amount of intergranular phase (volume content is less than 2%), Y
0.4Si
9.6Al
2.4O
1.2N
14.8Three-point bending strength be 515MPa and Yb
0.4Si
9.6Al
2.4O
1.2N
14.8Three-point bending strength be 525MPa, fracture toughness property is not less than 5.8MPam
1/2Method of attachment is the SPS method, and method of attachment and embodiment 14 differences are to be incubated 0~20min down at 1700 ℃ in the step 2, and other step is identical with embodiment 14 with parameter.
In the present embodiment, come out of the stove from beginning to weld weldment, the time spent is no more than 40min, compares with the pressure diffusion welding described in the technical background, has improved working efficiency widely.1700 ℃ down insulation 10min obtain the seam organization structures macro morphology as shown in Figure 3, microscopic appearance as shown in Figure 4, the bending strength of joint is with the variation relation of 1700 ℃ of following soaking times as described in Figure 5; Weldquality is good as can be known by Fig. 3-4, and with the lengthening of soaking time, the bending strength of weld seam increases as shown in Figure 5.
Embodiment 16: what present embodiment and embodiment 15 were different is: after step 2 naturally cools to room temperature with stove, place High Temperature Furnaces Heating Apparatus again, pressure<10Pa will be evacuated down to then in the High Temperature Furnaces Heating Apparatus, charging into nitrogen pressure to the stove again is 0.1MPa, be heated to 1700 ℃ with 30 ℃/min temperature rise rate then, high-temperature heat treatment 120min under 1700 ℃ of conditions stops heating then, naturally cools to room temperature with stove again.Other step and parameter are identical with embodiment 15.
After tested, strength of joint improves more than the 30MPa than untreated joint head intensity.Seam weave construction after present embodiment thermal treatment is as 6 and shown in Figure 7, and compares without the joint microstructure Fig. 3-4 before the pyroprocessing, can see that SiAlON crystal grain grows in seam, and then remedy the highly malleablized mechanism of joint, thereby improve strength of joint.
Embodiment 17: what present embodiment was different with embodiment is to be incubated 10min under 1600-1800 ℃ of condition, and other step is identical with embodiment 15 with parameter.
After tested, the strength of joint of the weldment after being connected slightly increases with the rising that connects temperature, all is higher than 530MPa, and maximum reaches 547MPa, greater than the intensity of mother metal.
Embodiment 18: present embodiment adopts the SPS method to connect to α-SiAlON pottery, β-SiAlON pottery.Described α-SiAlON pottery doped metal ion is Yb, and composition is described identical with embodiment 15; The chemical formula composition of β-SiAlON pottery is Si
4.8Al
1.2O
1.2N
6.8, its thing constitutes pure β-SiAlON mutually, and the intergranular phase content is not more than 2% volume ratio, and the three-point bending strength and the fracture toughness property of β-SiAlON pottery are respectively 900MPa and 11.2MPam
1/2Method of attachment and embodiment 15 differences are that step 2 is incubated 10min down at 1700 ℃.Other step is identical with concrete mode 15 with parameter.
The strength of joint of the weldment after after tested, present embodiment obtains to connect is 922MPa.
Embodiment 19: present embodiment is to two β-Si
3N
4Pottery adopts the SPS method to connect β-Si
3N
4Pottery is with α-Si
3N
4Powder is a raw material, and having added composition is 5% (weight) Y
2O
3With 2% (weight) Al
2O
3The sintering agent of weight ratio becomes technology with embodiment 15; β-Si
3N
4The thing of stupalith constitutes mutually with β-Si
3N
4Be main, contain the intergranular phase of about 7% volume ratio, three-point bending strength and fracture toughness property are respectively 790MPa and 8.2MPam
1/2The step of method of attachment is identical with embodiment 18 with parameter.
Adopt the mother metal of method for welding welding present embodiment, solder compositions is referring to volume 2 phases the 130th page the record in June the 23rd in 2002 of ceramic journal, in welding temperature is that 1600 ℃, weldment end force are to be incubated 30min under the condition of 5MPa, obtain strength of joint 632MPa, its strength of joint is less than the intensity of mother metal; The strength of joint of the weldment after after tested, present embodiment obtains to connect is not less than 817MPa; Its strength of joint is greater than strength of parent.
Embodiment 20: present embodiment is to SiAlON pottery and β-Si
3N
4Stupalith adopts the SPS method to connect, and described α-SiAlON pottery doped metal ion is Yb, and composition is described identical with embodiment 15; Described β-Si
3N
4Ceramics component is described identical with embodiment 19; The step of method of attachment is identical with embodiment 18 with parameter.
The strength of joint of the weldment after after tested, present embodiment obtains to connect is 796MPa.
Claims (10)
1.SiAlON pottery, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment is characterized in that SiAlON pottery, Si between pottery
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment is undertaken by following step between pottery: one, mother metal to be welded surface is polished with emery wheel whole, with ethanol flush away surface contamination and foreign material; Two, being connected of the mother metal to be welded that will handle through step 1 in the face of putting, the mould of packing into is placed in discharge plasma sintering (SPS) stove, to be evacuated down to pressure<6Pa in discharge plasma sintering (SPS) stove, charging into nitrogen to the interior pressure of discharge plasma sintering (SPS) stove again is 0.1~5MPa, increase the weldment end force when heating up then gradually, temperature rises to 700 ℃ of weldment end forces and reaches 1~100MPa, be heated to 1300~1900 ℃ with 5~200 ℃/min temperature rise rate in the time of pressurize, be incubated 0~90min again, stop heating, remove pressure, naturally cool to room temperature with stove again; SiAlON pottery, Si have promptly been finished
3N
4Pottery discharge plasma sintering of the same race or xenogeneic (SPS) connects; Wherein the described mother metal to be welded of step 1 is SiAlON pottery, Si
3N
4Same material or foreign material between pottery.
2. SiAlON pottery according to claim 1, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery is characterized in that the weldment end force is 5~80MPa pressure in the step 2.
3. SiAlON pottery according to claim 1, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery is characterized in that the weldment end force is 10~50MPa pressure in the step 2.
4. SiAlON pottery according to claim 1, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery is characterized in that the weldment end force is a 20MPa pressure in the step 2.
5. according to claim 1,2,3 or 4 described SiAlON potteries, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery is characterized in that being incubated 5~20min in the step 2 under 1400~1800 ℃ of conditions.
6. according to claim 1,2,3 or 4 described SiAlON potteries, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery is characterized in that being incubated 10min in the step 2 under 1700 ℃ of conditions.
7. SiAlON pottery according to claim 5, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery is characterized in that the described temperature rise rate of step 2 is 100 ℃/min.
8. according to claim 1,2,3,4 or 7 described SiAlON potteries, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery, it is characterized in that after step 2 naturally cools to room temperature with stove, again weldment is placed High Temperature Furnaces Heating Apparatus, pressure<10Pa will be evacuated down in the High Temperature Furnaces Heating Apparatus, charging into nitrogen pressure to the stove again is 0.1~0.5MPa, be heated to 1300~1900 ℃ with 5~100 ℃/min temperature rise rate then, high-temperature heat treatment 30~1800min under 1300~1900 ℃ of conditions, stop heating then, naturally cool to room temperature with stove again.
9. SiAlON pottery according to claim 8, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery, the temperature that it is characterized in that high-temperature heat treatment is 1500~1800 ℃.
10. SiAlON pottery according to claim 9, Si
3N
4The discharge plasma sintering of same material or foreign material (SPS) method of attachment between pottery, the time that it is characterized in that high-temperature heat treatment is 60~200min.
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CN103787663B (en) * | 2014-02-25 | 2015-03-11 | 丽水桉阳生物科技有限公司 | Multiphase high-strength high-thermal conductivity silicon nitride ceramic cutter material and cutter |
CN105081502B (en) * | 2015-09-14 | 2017-06-13 | 哈尔滨工业大学 | A kind of method of nitrogen treatment and its assistant brazing ceramic matric composite |
CN106825885B (en) * | 2017-02-24 | 2019-03-08 | 合肥工业大学 | A kind of connection method of TZM alloy and WRe alloy under electric field-assisted |
CN107081517B (en) * | 2017-06-28 | 2019-11-29 | 合肥工业大学 | A kind of law temperature joining method of TZM and WRe different alloys |
WO2022072705A2 (en) * | 2020-10-03 | 2022-04-07 | Heraeus Conamic North America Llc | Sintered ceramic body of large dimension and method of making |
CN116217240B (en) * | 2022-12-06 | 2024-02-02 | 广东工业大学 | Textured gradient ceramic composite material and preparation method and application thereof |
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CN1827279A (en) * | 2004-09-16 | 2006-09-06 | Esk制陶两合公司 | Method for the low-deformation diffusion-welding of ceramic components |
CN1903795A (en) * | 2006-08-02 | 2007-01-31 | 哈尔滨工业大学 | Method of low temperature active vacuum diffusion connecting ceramic |
CN101125759A (en) * | 2006-08-18 | 2008-02-20 | 中国科学院金属研究所 | Diffusion connection technique for ternary layered ceramic aluminum titanium carbide |
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CN1827279A (en) * | 2004-09-16 | 2006-09-06 | Esk制陶两合公司 | Method for the low-deformation diffusion-welding of ceramic components |
CN1903795A (en) * | 2006-08-02 | 2007-01-31 | 哈尔滨工业大学 | Method of low temperature active vacuum diffusion connecting ceramic |
CN101125759A (en) * | 2006-08-18 | 2008-02-20 | 中国科学院金属研究所 | Diffusion connection technique for ternary layered ceramic aluminum titanium carbide |
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