CN108264350A - A kind of preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target - Google Patents
A kind of preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target Download PDFInfo
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- CN108264350A CN108264350A CN201810250897.1A CN201810250897A CN108264350A CN 108264350 A CN108264350 A CN 108264350A CN 201810250897 A CN201810250897 A CN 201810250897A CN 108264350 A CN108264350 A CN 108264350A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HEOGEEMADXKTBU-UHFFFAOYSA-N [O].[Mn].[Ca].[La] Chemical compound [O].[Mn].[Ca].[La] HEOGEEMADXKTBU-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 98
- 238000005245 sintering Methods 0.000 claims abstract description 75
- 230000008569 process Effects 0.000 claims abstract description 38
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000013467 fragmentation Methods 0.000 claims abstract description 32
- 238000006062 fragmentation reaction Methods 0.000 claims abstract description 32
- 230000003068 static effect Effects 0.000 claims abstract description 32
- 238000003825 pressing Methods 0.000 claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 claims abstract description 29
- 239000004332 silver Substances 0.000 claims abstract description 29
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 claims abstract description 12
- 239000003292 glue Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 230000007704 transition Effects 0.000 claims description 137
- 238000000498 ball milling Methods 0.000 claims description 39
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 230000006835 compression Effects 0.000 claims description 18
- 238000007906 compression Methods 0.000 claims description 18
- 239000003755 preservative agent Substances 0.000 claims description 17
- 230000002335 preservative effect Effects 0.000 claims description 17
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000005187 foaming Methods 0.000 claims description 7
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 7
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012046 mixed solvent Substances 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 abstract description 10
- 230000007547 defect Effects 0.000 abstract description 7
- 239000011575 calcium Substances 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 230000008685 targeting Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 229910003410 La0.7Ca0.3MnO3 Inorganic materials 0.000 description 8
- 230000005611 electricity Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000035945 sensitivity Effects 0.000 description 6
- 230000009514 concussion Effects 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 238000005538 encapsulation Methods 0.000 description 4
- 229910002269 La1–xCaxMnO3 Inorganic materials 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001182 laser chemical vapour deposition Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002887 superconductor Substances 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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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The present invention discloses a kind of preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target, belongs to field of ceramic preparation technology.Specifically include following steps：Collosol craft, gel process, dry glue technique, a fragmentation technique, a calcine technology mix silver process, powder static pressure technique, secondary clacining technique, secondary fragmentation technique, pre-embossed technique, whole mould static pressure technique, three times calcine technology；The method of the invention can be mixed and be permeated by liquid phase and is sintered, and improve Ag doping effects, doping loss is greatly reduced so that practical doping ratio strengthens the anisotropy of ceramic target close to calculation amount；With reference to non-oxide sintering process so that La1‑x Ca x MnO3Matrix and Ag elements are not oxidized before doping is not completed, and then improve doping effect；With reference to isostatic cool pressing technique, permeating and generating multiaxial stress in pressing process, target can be conducive to and make substantially to eliminate defect(ive) structure while preferential growth, so that ceramic target has strong anisotropy.
Description
Technical field
The present invention relates to a kind of preparation methods of anisotropy lanthanum calcium manganese oxygen base ceramic target, belong to ceramics processing neck
Domain.
Background technology
La1-xCaxMnO3 is the doped rare-earth manganites of perovskite structure.With giant magnetoresistance effect and laser induced chemical vapor deposition electricity
Effect is pressed, can be used to make giant magnetoresistance bolograph, electrooptical device, high density storage head, contactless magnetic resistance and open
Pass, magnetic susceptibility sensor, thermo-electric device etc., therefore the research interest of numerous scholars is caused, become strong after high-temperature superconductor
The another research hotspot of associated material system.Current La1-xCaxMnO3 architectural studies emphasis is synthetically prepared for doping Ag, and one
Can auxiliary ceramic target preferential growth is presented in growth course so that target anisotropy is strengthened, greatly improve target
The electric property of material；Two can be because of anisotropic enhancing, and the temperature sensitive performance of electricity for greatly improving material.And current system
There is the common faults of the following aspects mostly in standby technique：（1）It is mixed mostly using granulating silver powder in the prior art
Sintering, achievees the purpose that doping by solid phase reaction, although can be by controlling the grain size of silver powder come improvement effect, solid phase be anti-
The defects of answering still exists, and doping effect is poor, and doping loss is too big, and doping ratio is far below calculation amount；（2）In current technology
Which kind of either adulterated using mode, without anti-oxidation measure, one being La1-xCaxMnO3 basis materials by oxidation shape
Into after stable state, Ag elements are not easy doping and enter, and two being that Ag factors itself are aoxidized, and it is poor to lead to adulterate effect, Wu Fayou
Effect is entered in basis material；（3）In existing technological operation, using conventional compacting means, directional stress can be generally generated, one
Make preferential growth in follow-up sintering to be unfavorable for target, two can not substantially eliminate defect.So it in view of the above-mentioned problems, sets
Meter, which develops a kind of preparation process of strong anisotropy (LaxCa1-xMnO3) Agy ceramic targets, becomes current urgent need.
Invention content
For problems of the prior art, the purpose of the present invention is to provide a kind of anisotropic ceramics targets
(LaxCa1-xMnO3)·AgyPreparation method, specifically include following steps：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into (LaxCa1-xMnO3)·AgyStoichiometry match
Than being weighed, it is subsequently poured into mixing vessel, mixed solvent carrier is made using methanol, ethylene glycol makees dispersant, is obtained after mixing
To transition object I；Wherein, XIt is 0.1 ~ 0.3 for 0.66 ~ 0.75, y.
（2）Gel process：By step（1）Gained transition object I is placed in 75 DEG C ~ 90 DEG C environment and steams, and obtains transition object II.
（3）Dry glue technique：By step（2）Gained transition object II, which is placed in 110 DEG C ~ 130 DEG C environment, is dehydrated foaming, obtains
Transition object III.
（4）Fragmentation technique：To step（3）Gained transition object III makees ball milling fragmentation and handles to obtain transition object IV；Pass through
Fragmentation so that particle size size is sufficiently small, and can guarantee can completely volatilize the impurity of non-ingredient during subsequent primary calcining
Fall, and enough volatilization channels can be formed.
（5）Calcine technology：To step（4）Gained transition object IV, which is made once to calcine, obtains transition object V；By non-oxygen
Change and be unlikely to generate oxide layer while sintering enables to the impurity component in transition object IV to be vapored away completely, cause follow-up
Silver element can not adulterate and enter material system.
（6）Mix silver process：Silver paste is uniformly applied on the grinding bead of ball mill on the inside of ball milling tank skin, then will walked
Suddenly（5）Gained transition object V pours into ball grinder and starts ball milling, obtains transition object VI；It can ensure enough silver pastes by the technique
It is applied on transition object V, while side coated side fragmentation can guarantee overall coat largest surface area.
（7）Powder static pressure technique：By step（6）Gained transition object VI obtains transition object VII after carrying out isostatic cool pressing；The step
Suddenly it can ensure that transition object VI by comprehensive extruding force, forms infiltration interface under prolonged condition of high voltage, is follow-up
Secondary clacining lays the foundation.
（8）Secondary clacining technique：By step（7）Gained transition object VII carries out secondary clacining, obtains transition object VIII；By this
Step is sintered, and can ensure that the band silver element permeable formation of very thin thickness is entered in basis material, and vacuum state can guarantee silver
Element is not aoxidized largely so that silver element is really adulterated.
（9）Secondary fragmentation technique：By ball mill to step（8）Gained transition object VIII carries out ball milling fragmentation and obtains transition object
Ⅸ；By the complete product refinement mixing of ingredient, ensure that the ingredient of follow-up ceramic target entirety is uniform.
（10）Pre-embossed technique：By step（9）Gained transition object Ⅸ is pressed into pre- mould target.
（11）Whole mould static pressure technique：Step（10）The pre- mould target of gained carries out isostatic cool pressing and obtains whole mould target；The step can protect
Ceramic target is demonstrate,proved by comprehensive extruding force, consistency is greatly improved, reduces the probability that defect generates, be when subsequently calcining three times
Preferential growth lay the foundation.
（12）Calcine technology three times：To step（11）Gained end mould target carries out oxygen-enriched sintering, obtains anisotropy
(LaxCa1-xMnO3)·AgyCeramic target；Obtain that there is anisotropic ceramic target by preferential growth.
Preferably, step of the present invention（4）IV grain size of transition object that middle ball milling fragmentation is handled is less than 0.1mm.
Preferably, step of the present invention（5）The condition once calcined is：Vacuum degree is less than 500Pa, and sintering temperature is
480 DEG C ~ 500 DEG C, sintering time is 6h ~ 8h.
Preferably, step of the present invention（6）The usage amount of middle silver paste is the 105% ~ 107% of true calculation amount, and silver paste viscosity is
1.5CPS~2.5 CPS；Ball milling condition is：Rotational speed of ball-mill is the r/min of 300r/min ~ 600, a length of 6 ~ 8h during ball milling.
Preferably, step of the present invention（7）The detailed process of middle isostatic cool pressing is：Gained transition object VI is poured over preservative film
On, concussion tiling makees transition object VI by ultrasonic plate, the rear package that folds is encapsulated again with preservative film and TR thin rubber bag successively, right
Thinner package rubber bag vacuumizes, and will be submerged into vacuum state TR thin rubber bag in isostatic cool pressing sump and carry out static pressure；Static pressure process
It is operated for staged pressurize, pressure value is 170Mpa ~ 210Mpa, and compressions total time is the min of 40min ~ 180.
Preferably, step of the present invention（8）Described in the condition of secondary clacining be：Vacuum degree is less than 500Pa, and sintering temperature is
400 DEG C ~ 450 DEG C, a length of 12h ~ 15h during sintering.
Preferably, step of the present invention（9）Middle Ⅸ grain size of gained transition object is less than 0.5mm.
Preferably, step of the present invention（10）Described in pressing process pressure for 8Mpa ~ 13Mpa, compression total duration is
10min ~ 20 min。
Preferably, step of the present invention（11）The detailed process of the isostatic cool pressing is：Preservative film and TR thin rubber bag are used successively
It encapsulates, thinner package rubber bag is vacuumized by hytor, isostatic cool pressing sump will be submerged into vacuum state TR thin rubber bag
Interior progress static pressure operation, the static pressure process are operated for staged pressurize, and pressure value is 230Mpa ~ 250Mpa, when being pressurized total
The min of a length of 15min ~ 20.
Preferably, step of the present invention（12）The condition of the oxygen-enriched sintering is：Sintering temperature is 1350 DEG C ~ 1450 DEG C, is burnt
A length of 12h ~ 16h during knot, flowing oxygen pressure is 0.01Mpa ~ 0.07Mpa.
Compared with prior art, it is an advantage of the invention that：
（1）Present invention process can be mixed and be permeated by liquid phase and is sintered, and improve Ag doping effects, doping loss is greatly reduced,
Cause practical doping ratio close to calculation amount, and then strengthen the anisotropy of ceramic target.
（2）Present invention process can combine non-oxide sintering process so that La1-x Ca x MnO3Matrix and Ag elements be not complete
It is not oxidized before into doping, and then improve doping effect.
（3）Present invention process combination isostatic cool pressing technique is permeating and is generating multiaxial stress in pressing process, can be conducive to
Target is made substantially to eliminate defect(ive) structure while preferential growth, so that ceramic target has strong anisotropy.
Description of the drawings
Fig. 1 is the target electrical performance testing figure of embodiment 1；
Fig. 2 is the target electrical performance testing figure of comparative example 1；
Fig. 3 is the target electrical performance testing figure of comparative example 2；
Fig. 4 is the target electrical performance testing figure of comparative example 3.
Specific embodiment：
The present invention will be described in detail with reference to the accompanying drawings and examples, these embodiments are only because the mesh that exemplary illustrates
, and it is not intended to limit the present invention.
Embodiment 1
A kind of strong anisotropy (La0.7Ca0.3MnO3)·Ag0.2The preparation process of ceramic target, specifically includes following steps：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into quality proportioning 6:1:6:19 pour into mixing vessel,
Mixed solvent carrier is made using methanol, dispersant is made using ethylene glycol, is mixed to get transition object I.
（2）Gel process：By step（1）Gained transition object I is positioned over 80 DEG C of environment and steams, and obtains transition object II.
（3）Dry glue technique：By step（2）Gained transition object II is positioned over 120 DEG C of environment and makees dehydration foaming, obtains transition
Object III.
（4）Fragmentation technique：By ball mill to step（3）Gained transition object III makees ball milling fragmentation and obtains transition object
Ⅳ（Grain size is less than 0.1mm）.
（5）Calcine technology：By vacuum sintering furnace to step（4）Gained transition object IV, which is made once to calcine, obtains transition
Object V；The vacuum degree once calcined need to be less than 500Pa, and sintering temperature is 490 DEG C, a length of 7h during sintering.
（6）Mix silver process：The amount of being intended to silver paste is uniformly applied on the grinding bead of ball mill and ball milling tank skin inside, after
By step（5）Gained transition object V, which is poured into ball grinder, makees ball milling operation, obtains transition object VI；The amount of plan is calculated to be true
The 106% of amount, silver paste range of viscosities are 2.0 CPS, and the rotational speed of ball-mill of the ball milling operation is 450 r/min, ball milling duration
For 7h.
（7）Powder static pressure technique：By step（6）Gained transition object VI is poured on preservative film, by ultrasonic plate to transition
Object VI makees concussion tiling, and the rear package that folds is encapsulated again with preservative film and TR thin rubber bag successively, by hytor to thinner package rubber
Poly-bag makees vacuum operation, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag and make static pressure operation, and obtain transition object
Ⅶ；The static pressure operation can make staged pressurize operation, range of pressure values 190Mpa, compression total duration ranging from 100 min.
（8）Secondary clacining technique：By step（7）Gained transition object VII is poured out from encapsulation, by vacuum sintering furnace to mistake
It crosses object VII and makees secondary clacining, obtain transition object VIII；The secondary clacining vacuum degree need to be less than 500Pa, and sintering temperature is 430 DEG C,
A length of 14h during sintering.
（9）Secondary fragmentation technique：By ball mill to step（8）Gained transition object VIII makees ball milling fragmentation and obtains transition object Ⅸ
（Grain size is less than 0.5mm）.
（10）Pre-embossed technique：By type mechanical tableting machine by step（9）Gained transition object Ⅸ is pressed into pre- mould target；It is described
The range of pressure values used is suppressed as 10Mpa, compression total duration ranging from 15min.
（11）Whole mould static pressure technique：By step（10）The pre- mould target of gained is encapsulated successively with preservative film and TR thin rubber bag, is led to
Cross hytor and vacuum operation made to thinner package rubber bag, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag make it is quiet
Operation is pressed, obtains whole mould target；The static pressure operation can carry out staged pressurize operation, pressure value 240Mpa, compression total duration
Ranging from 18min.
（12）Calcine technology three times：By atmosphere sintering furnace to step（11）Gained end mould target makees oxygen-enriched sintering, obtains strong
Anisotropy (La0.7Ca0.3MnO3)·Ag0.2Ceramic target.The sintering temperature of the oxygen-enriched sintering is 1400 DEG C, and when sintering is a length of
14h, flowing oxygen pressure is 0.04Mpa.
The target electrical performance testing that the present embodiment 1 is prepared is as shown in Figure 1, by can be seen that it perpendicular to target in figure
To magnetic field environment in, during positioned at 256.68K, TCR values are 33.67%, and in magnetic field environment of the level in targeting, are located at
During 257.21K, TCR values are 46.35%.In the case of understanding that electricity sensitive temperature point is not much different, not only electric property is big
Width improves, and electrical sensitivity energy difference, that is, TCR differences are improved to 12.68%, and it is strong respectively to different to can determine whether that the ceramic target has
Property.
Embodiment 2
A kind of strong anisotropy (La0.7Ca0.3MnO3)·Ag0.2The preparation process of ceramic target, specifically includes following steps：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into quality proportioning 6:1:6:19 pour into mixing vessel,
Mixed solvent carrier is made using methanol, dispersant is made using ethylene glycol, is mixed to get transition object I.
（2）Gel process：By step（1）Gained transition object I is positioned over 75 DEG C of environment and steams, and obtains transition object II.
（3）Dry glue technique：By step（2）Gained transition object II is positioned over 110 DEG C of environment and makees dehydration foaming, obtains transition
Object III.
（4）Fragmentation technique：By ball mill to step（3）Gained transition object III makees ball milling fragmentation and obtains transition object
Ⅳ（Grain size is less than 0.1mm）.
（5）Calcine technology：By vacuum sintering furnace to step（4）Gained transition object IV, which is made once to calcine, obtains transition
Object V；The vacuum degree once calcined need to be less than 500Pa, and sintering temperature is 480 DEG C, a length of 6h during sintering.
（6）Mix silver process：The amount of being intended to silver paste is uniformly applied on the grinding bead of ball mill and ball milling tank skin inside, after
By step（5）Gained transition object V, which is poured into ball grinder, makees ball milling operation, obtains transition object VI；The amount of plan is calculated to be true
The 105% of amount, silver paste range of viscosities are 1.5CPS, and the rotational speed of ball-mill of the ball milling operation is 300r/min, and when ball milling is a length of
6h。
（7）Powder static pressure technique：By step（6）Gained transition object VI is poured on preservative film, by ultrasonic plate to transition
Object VI makees concussion tiling, and the rear package that folds is encapsulated again with preservative film and TR thin rubber bag successively, by hytor to thinner package rubber
Poly-bag makees vacuum operation, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag and make static pressure operation, and obtain transition object
Ⅶ；The static pressure operation can make staged pressurize operation, range of pressure values 170Mpa, compression total duration ranging from 40min.
（8）Secondary clacining technique：By step（7）Gained transition object VII is poured out from encapsulation, by vacuum sintering furnace to mistake
It crosses object VII and makees secondary clacining, obtain transition object VIII；The secondary clacining vacuum degree need to be less than 500Pa, and sintering temperature is 400 DEG C,
A length of 12h during sintering.
（9）Secondary fragmentation technique：By ball mill to step（8）Gained transition object VIII makees ball milling fragmentation and obtains transition object Ⅸ
（Grain size is less than 0.5mm）.
（10）Pre-embossed technique：By type mechanical tableting machine by step（9）Gained transition object Ⅸ is pressed into pre- mould target；It is described
The range of pressure values used is suppressed as 8Mpa, compression total duration ranging from 10min.
（11）Whole mould static pressure technique：By step（10）The pre- mould target of gained is encapsulated successively with preservative film and TR thin rubber bag, is led to
Cross hytor and vacuum operation made to thinner package rubber bag, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag make it is quiet
Operation is pressed, obtains whole mould target；The static pressure operation can carry out staged pressurize operation, pressure value 230Mpa, compression total duration
Ranging from 15min.
（12）Calcine technology three times：By atmosphere sintering furnace to step（11）Gained end mould target makees oxygen-enriched sintering, obtains strong
Anisotropy (La0.7Ca0.3MnO3)·Ag0.2Ceramic target.The sintering temperature of the oxygen-enriched sintering is 1350 DEG C, and when sintering is a length of
12h, flowing oxygen pressure is 0.01Mpa.
In the magnetic field environment perpendicular to targeting, TCR values are the target electric property that the present embodiment 2 is prepared
25.66%, and in magnetic field environment of the level in targeting, TCR values are 37.53%.Understand that electrical sensitivity energy difference, that is, TCR is poor
Value is improved to 11.87%, can determine whether that the ceramic target has strong anisotropy.
Embodiment 3
A kind of strong anisotropy (La0.7Ca0.3MnO3)·Ag0.2The preparation process of ceramic target, specifically includes following steps：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into quality proportioning 6:1:6:19 pour into mixing vessel,
Mixed solvent carrier is made using methanol, dispersant is made using ethylene glycol, is mixed to get transition object I.
（2）Gel process：By step（1）Gained transition object I is positioned over 90 DEG C of environment and steams, and obtains transition object II.
（3）Dry glue technique：By step（2）Gained transition object II is positioned over 130 DEG C of environment and makees dehydration foaming, obtains transition
Object III.
（4）Fragmentation technique：By ball mill to step（3）Gained transition object III makees ball milling fragmentation and obtains transition object
Ⅳ（Grain size is less than 0.1mm）.
（5）Calcine technology：By vacuum sintering furnace to step（4）Gained transition object IV, which is made once to calcine, obtains transition
Object V；The vacuum degree once calcined need to be less than 500Pa, and sintering temperature is 500 DEG C, a length of 8h during sintering.
（6）Mix silver process：The amount of being intended to silver paste is uniformly applied on the grinding bead of ball mill and ball milling tank skin inside, after
By step（5）Gained transition object V, which is poured into ball grinder, makees ball milling operation, obtains transition object VI；The amount of plan is calculated to be true
The 107% of amount, silver paste range of viscosities are 2.5 CPS, and the rotational speed of ball-mill of the ball milling operation is 600 r/min, ball milling duration
For 8h.
（7）Powder static pressure technique：By step（6）Gained transition object VI is poured on preservative film, by ultrasonic plate to transition
Object VI makees concussion tiling, and the rear package that folds is encapsulated again with preservative film and TR thin rubber bag successively, by hytor to thinner package rubber
Poly-bag makees vacuum operation, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag and make static pressure operation, and obtain transition object
Ⅶ；The static pressure operation can make staged pressurize operation, range of pressure values 210Mpa, compression total duration ranging from 180 min.
（8）Secondary clacining technique：By step（7）Gained transition object VII is poured out from encapsulation, by vacuum sintering furnace to mistake
It crosses object VII and makees secondary clacining, obtain transition object VIII；The secondary clacining vacuum degree need to be less than 500Pa, and sintering temperature is 450 DEG C,
A length of 15h during sintering.
（9）Secondary fragmentation technique：By ball mill to step（8）Gained transition object VIII makees ball milling fragmentation and obtains transition object Ⅸ
（Grain size is less than 0.5mm）.
（10）Pre-embossed technique：By type mechanical tableting machine by step（9）Gained transition object Ⅸ is pressed into pre- mould target；It is described
The range of pressure values used is suppressed as 13Mpa, compression total duration ranging from 20 min.
（11）Whole mould static pressure technique：By step（10）The pre- mould target of gained is encapsulated successively with preservative film and TR thin rubber bag, is led to
Cross hytor and vacuum operation made to thinner package rubber bag, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag make it is quiet
Operation is pressed, obtains whole mould target；The static pressure operation can carry out staged pressurize operation, pressure value 250Mpa, compression total duration
Ranging from 20 min.
（12）Calcine technology three times：By atmosphere sintering furnace to step（11）Gained end mould target makees oxygen-enriched sintering, obtains strong
Anisotropy (La0.7Ca0.3MnO3)·Ag0.2Ceramic target.The sintering temperature of the oxygen-enriched sintering is 1450 DEG C, and when sintering is a length of
16h, flowing oxygen pressure is 0.07Mpa.
In the magnetic field environment perpendicular to targeting, TCR values are the target electric property that the present embodiment 3 is prepared
27.56%, and in magnetic field environment of the level in targeting, TCR values are 38.45%.Understand that electrical sensitivity energy difference, that is, TCR is poor
Value is improved to 10.89%, can determine whether that the ceramic target has strong anisotropy.
It can be seen that the silver paste medium that Ag elements use from the technique of embodiment 1,2,3 so that it is mixed with basis material
Uniformly and it is tightly combined, it is sufficiently thin in combination with layer, adulterate its infiltration by non-oxide sintering, in target pressing process
It is made to generate multiaxial stress by isostatic cool pressing technique, is conducive to target and makees substantially to eliminate defect(ive) structure while preferential growth,
Finally complete to prepare by oxygen-enriched sintering.
Comparative example 1
This comparative example prepares (La using following steps0.7Ca0.3MnO3)·Ag0.2Ceramic target：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into quality proportioning 6:1:6:19 pour into mixing vessel,
Mixed solvent carrier is made using methanol, dispersant is made using ethylene glycol, is mixed to get transition object I.
（2）Gel process：By step（1）Gained transition object I is positioned over 80 DEG C of environment and steams, and obtains transition object II.
（3）Dry glue technique：By step（2）Gained transition object II is positioned over 120 DEG C of environment and makees dehydration foaming, obtains transition
Object III.
（4）Fragmentation technique：By ball mill to step（3）Gained transition object III makees ball milling fragmentation and obtains transition object
IV, IV grain size of transition object is 0.08mm.
（5）Calcine technology：By normal sintering stove to step（4）Gained transition object IV, which is made once to calcine, obtains transition
Object V, sintering temperature are 490 DEG C, a length of 7h during sintering.
（6）Mix silver process：By the silver powder of 200 mesh grain sizes（Specially 0.26g）It is doped into cross in object five and is ground mixing,
Obtain transition object VI.
（7）Pressing process：By type mechanical tableting machine by step（6）Gained transition object VI is pressed into target, suppresses the pressure of use
Force value is 12Mpa, compression total duration ranging from 18 min.
（8）Secondary clacining technique：By normal sintering stove to step（7）Gained target is sintered, and is obtained
(La0.7Ca0.3MnO3)·Ag0.2Ceramic target, sintering temperature are 1400 DEG C, a length of 14h during sintering.
This comparative example 1 is the (La being prepared using existing routine techniques0.7Ca0.3MnO3)·Ag0.2The electricity of ceramic target
Performance test is as shown in Fig. 2, TCR values in Fig. 2 are ceramic target under orthogonal magnetic field state, itself electrical sensitivity energy
Feedback, by can be seen that it in figure in the magnetic field environment perpendicular to targeting, during positioned at 266.85K, TCR values are 17.27%,
And in magnetic field environment of the level in targeting, during positioned at 268.5K, TCR values are 19.87%.Understand electricity sensitive temperature point phase
In the case that difference is little, electrical sensitivity energy difference, that is, TCR differences are only 2.6%.So it can determine whether the ceramic target anisotropy
It is low.
Comparative example 2
This comparative example prepares (La using following steps0.7Ca0.3MnO3)·Ag0.2Ceramic target：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into quality proportioning 6:1:6:19 pour into mixing vessel,
Mixed solvent carrier is made using methanol, dispersant is made using ethylene glycol, is mixed to get transition object I.
（2）Gel process：By step（1）Gained transition object I is positioned over 80 DEG C of environment and steams, and obtains transition object II.
（3）Dry glue technique：By step（2）Gained transition object II is positioned over 120 DEG C of environment and makees dehydration foaming, obtains transition
Object III.
（4）Fragmentation technique：By ball mill to step（3）Gained transition object III makees ball milling fragmentation and obtains transition object
IV, IV grain size of transition object is 0.08mm.
（5）Calcine technology：By vacuum sintering furnace to step（4）Gained transition object IV, which is made once to calcine, obtains transition
Object V, sintering temperature are 490 DEG C, a length of 7h, vacuum degree 450Pa during sintering.
（6）Mix silver process：The amount of being intended to silver paste is uniformly applied on the grinding bead of ball mill and ball milling tank skin inside, after
By step（5）Gained transition object V, which is poured into ball grinder, makees ball milling operation, obtains transition object VI, amount of plan 106%, silver paste is glued
Spend ranging from 2CPS.The rotational speed of ball-mill of ball milling operation is 450 r/min, a length of 7h during ball milling.
（7）Powder static pressure technique：By step（6）Gained transition object VI is poured on preservative film, by ultrasonic plate to transition
Object VI makees concussion tiling, and the rear package that folds is encapsulated again with preservative film and TR thin rubber bag successively, by hytor to thinner package rubber
Poly-bag makees vacuum operation, will be submerged into isostatic cool pressing sump in vacuum state TR thin rubber bag and make static pressure operation, and obtain transition object
VII, staged pressurize operation, range of pressure values 190Mpa, compression total duration ranging from 110 min are made in static pressure operation.
（8）Secondary clacining technique：By step（7）Gained transition object VII is poured out from encapsulation, by vacuum sintering furnace to mistake
It crosses object VII and makees secondary clacining, obtain transition object VIII, sintering temperature is 425 DEG C, and a length of 13.5h during sintering, vacuum degree is 450 Pa.
（9）Secondary fragmentation technique：By ball mill to step（8）Gained transition object VIII makees ball milling fragmentation and obtains transition object
Ⅸ, Ⅸ grain size of transition object is 0.4mm.
（10）Pressing process：By type mechanical tableting machine by step（9）Gained transition object Ⅸ is pressed into target, suppresses the pressure of use
Force value is 12Mpa, compression total duration ranging from 18 min.
（11）Calcine technology three times：By atmosphere sintering furnace to step（10）Gained target makees oxygen-enriched sintering, obtain it is strong respectively to
The opposite sex (LaxCa1-xMnO3)·AgyCeramic target, sintering temperature are 1400 DEG C, a length of 14h during sintering, and flowing oxygen pressure is 0.04Mpa.
This comparative example 2 is to combine the techniques such as solid-liquid mixing, non-oxide infiltration sintering on the basis of current art to be prepared
(La0.7Ca0.3MnO3)·Ag0.2Ceramic target can be seen that the silver paste medium that Ag elements use so that itself and matrix from technique
Material is uniformly mixed and is tightly combined, sufficiently thin in combination with layer, adulterates its infiltration by non-oxide sintering, finally logical
Oxygen-enriched sintering is crossed to complete to prepare；The target electrical performance testing is as shown in figure 3, by can be seen that it perpendicular to targeting in Fig. 3
In magnetic field environment, during positioned at 260.76K, TCR values are 29.37%, and in magnetic field environment of the level in targeting, it is located at
During 261.4K, TCR values are 33.7%.In the case of understanding that electricity sensitive temperature point is not much different, not only electric property improves
, and electrical sensitivity energy difference, that is, TCR differences are improved to 4.33%, the ceramic target is respectively to different for can determine whether more conventional technique
Property improve.
Comparative example 3
The present embodiment step is according to 1 process implementing of embodiment, but in step（11）Described in compression total duration exceed the upper limit
Range.The target electrical performance testing is as shown in figure 4, by can be seen that it in the magnetic field environment perpendicular to targeting, is located in Fig. 4
During 244.79K, TCR values are 48.06%, and in magnetic field environment of the level in targeting, during positioned at 245.88K, TCR values are
49.95%.In the case of understanding that electricity sensitive temperature point is not much different, although electric property greatly improved, electricity is sensitive
Performance difference, that is, TCR differences are reduced to 1.89%, this is because pressurize is fine and close with that can strengthen target under High Voltage state for a long time
Degree.Defect is reduced, improves electric property, but also results in glass on the structure cell interface of ceramic target inside and mutually increases, causes subsequently to select
Tachyauxesis is obstructed, and can not form strong anisotropy, therefore can determine whether that the ceramic target anisotropy is low.
The ceramic target anisotropy comparing result of embodiment 1,2,3 and comparative example 1,2,3 is as shown in table 1, can by table 1
To find out that the present invention can make on the basis of sol gel process with reference to solid-liquid mixing, isostatic cool pressing and non-oxide infiltration sintering process
It is standby to obtain strong anisotropic (LaxCa1-xMnO3)·AgyIt is big to be embodied in electric property directional difference for ceramic target.
The different embodiments of table 1 and comparative example ceramic target anisotropy comparing result
Claims (10)
1. a kind of preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target, it is characterised in that：Specifically include following steps：
（1）Collosol craft：Lanthanum nitrate, calcium nitrate, manganese nitrate and citric acid are pressed into (LaxCa1-xMnO3)·AgyStoichiometry match
Than being weighed, it is subsequently poured into mixing vessel, mixed solvent carrier is made using methanol, ethylene glycol makees dispersant, is obtained after mixing
To transition object I；Wherein, XIt is 0.1 ~ 0.3 for 0.66 ~ 0.75, y；
（2）Gel process：By step（1）Gained transition object I is placed in 75 DEG C ~ 90 DEG C environment and steams, and obtains transition object II；
（3）Dry glue technique：By step（2）Gained transition object II, which is placed in 110 DEG C ~ 130 DEG C environment, is dehydrated foaming, obtains transition
Object III；
（4）Fragmentation technique：To step（3）Gained transition object III makees ball milling fragmentation and handles to obtain transition object IV；
（5）Calcine technology：To step（4）Gained transition object IV, which is made once to calcine, obtains transition object V；
（6）Mix silver process：Silver paste is uniformly applied on the grinding bead of ball mill and ball milling tank skin on the inside of, then by step
（5）Gained transition object V pours into ball grinder and starts ball milling, obtains transition object VI；
（7）Powder static pressure technique：By step（6）Gained transition object VI obtains transition object VII after carrying out isostatic cool pressing；
（8）Secondary clacining technique：By step（7）Gained transition object VII carries out secondary clacining, obtains transition object VIII；
（9）Secondary fragmentation technique：By ball mill to step（8）Gained transition object VIII carries out ball milling fragmentation and obtains transition object Ⅸ；
（10）Pre-embossed technique：By step（9）Gained transition object Ⅸ is pressed into pre- mould target；
（11）Whole mould static pressure technique：Step（10）The pre- mould target of gained carries out isostatic cool pressing and obtains whole mould target；
（12）Calcine technology three times：To step（11）Gained end mould target carries out oxygen-enriched sintering, obtains anisotropy (LaxCa1- xMnO3)·AgyCeramic target.
2. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（4）
IV grain size of transition object that middle ball milling fragmentation is handled is less than 0.1mm.
3. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（5）
The condition once calcined is：Vacuum degree is less than 500Pa, and sintering temperature is 480 DEG C ~ 500 DEG C, and sintering time is 6h ~ 8h.
4. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（6）
The usage amount of middle silver paste is the 105% ~ 107% of true calculation amount, and silver paste viscosity is the CPS of 1.5CPS ~ 2.5；Ball milling condition is：Ball
Mill rotating speed is the r/min of 300r/min ~ 600, a length of 6 ~ 8h during ball milling.
5. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（7）
The detailed process of middle isostatic cool pressing is：Gained transition object VI is poured on preservative film, transition object VI is shaken by ultrasonic plate
Paving is wiped out, the rear package that folds is encapsulated again with preservative film and TR thin rubber bag successively, and thinner package rubber bag is vacuumized, will be in vacuum
State TR thin rubber bag, which is submerged into isostatic cool pressing sump, carries out static pressure；Static pressure process is operated for staged pressurize, and pressure value is
170Mpa ~ 210Mpa, compression total time are the min of 40min ~ 180.
6. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（8）
Described in the condition of secondary clacining be：Vacuum degree is less than 500Pa, and sintering temperature is 400 DEG C ~ 450 DEG C, and a length of 12h during sintering ~
15h。
7. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（9）
Middle Ⅸ grain size of gained transition object is less than 0.5mm.
8. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（10）
Described in pressing process pressure for 8Mpa ~ 13Mpa, compression total duration is the min of 10min ~ 20.
9. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step（11）
The detailed process of the isostatic cool pressing is：It is encapsulated successively with preservative film and TR thin rubber bag, by hytor to encapsulating TR thin rubber
Bag vacuumizes, and will be submerged into vacuum state TR thin rubber bag in isostatic cool pressing sump and carry out static pressure operation, and the static pressure process is
Staged pressurize operates, and pressure value is 230Mpa ~ 250Mpa, and compression total duration is the min of 15min ~ 20.
10. the preparation method of anisotropy lanthanum calcium manganese oxygen base ceramic target according to claim 1, it is characterised in that：Step
（12）The condition of the oxygen-enriched sintering is：Sintering temperature is 1350 DEG C ~ 1450 DEG C, and a length of 12h ~ 16h during sintering flows oxygen pressure
For 0.01Mpa ~ 0.07Mpa.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475465A (en) * | 2003-07-04 | 2004-02-18 | 清华大学 | Zinc aluminium oxide ceramic target material suface indium coating method |
| CN1785906A (en) * | 2005-11-04 | 2006-06-14 | 北京工业大学 | Preparation method of lanthanum calcium manganese oxygen functional ceramic |
| JP2011192740A (en) * | 2010-03-12 | 2011-09-29 | Sumitomo Metal Electronics Devices Inc | Ceramic substrate |
| CN104651784A (en) * | 2015-03-13 | 2015-05-27 | 福建省诺希科技园发展有限公司 | Manufacturing method of carbon-silver composite target for curved touch screen |
| CN107285769A (en) * | 2017-05-03 | 2017-10-24 | 昆明理工大学 | A kind of preparation method of high TCR polycrystalline ceramics |
-
2018
- 2018-03-26 CN CN201810250897.1A patent/CN108264350B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475465A (en) * | 2003-07-04 | 2004-02-18 | 清华大学 | Zinc aluminium oxide ceramic target material suface indium coating method |
| CN1785906A (en) * | 2005-11-04 | 2006-06-14 | 北京工业大学 | Preparation method of lanthanum calcium manganese oxygen functional ceramic |
| JP2011192740A (en) * | 2010-03-12 | 2011-09-29 | Sumitomo Metal Electronics Devices Inc | Ceramic substrate |
| CN104651784A (en) * | 2015-03-13 | 2015-05-27 | 福建省诺希科技园发展有限公司 | Manufacturing method of carbon-silver composite target for curved touch screen |
| CN107285769A (en) * | 2017-05-03 | 2017-10-24 | 昆明理工大学 | A kind of preparation method of high TCR polycrystalline ceramics |
Non-Patent Citations (1)
| Title |
|---|
| 胡振江等: "镧钙锰氧陶瓷转变温度各向异性的研究", 《人工晶体学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451961A (en) * | 2019-08-23 | 2019-11-15 | 昆明理工大学 | A kind of preparation method of Ag doping lanthanum calcium manganese oxygen polycrystalline ceramics target |
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