CN1203209A - Process for preparing aluminium nitride whisker - Google Patents
Process for preparing aluminium nitride whisker Download PDFInfo
- Publication number
- CN1203209A CN1203209A CN 98103409 CN98103409A CN1203209A CN 1203209 A CN1203209 A CN 1203209A CN 98103409 CN98103409 CN 98103409 CN 98103409 A CN98103409 A CN 98103409A CN 1203209 A CN1203209 A CN 1203209A
- Authority
- CN
- China
- Prior art keywords
- whisker
- aluminium nitride
- powder
- aln
- mineralizer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 50
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 230000001089 mineralizing effect Effects 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 34
- 239000002245 particle Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 241000209456 Plumbago Species 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005354 coacervation Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- -1 CaCO 3 Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A process for preparing crystal whisker of aluminium nitride includes such steps as mixing Al2O3 with graphite powder or activated carbon, addition of mineralizing agent and alcohol, stirring in ball grinder, dry pressing to obtain blank, heating to temp. higher than 1500 deg.C in nitrogen atmosphere, keeping the temp for a certain time to synthesize crystal whisker of aluminium nitride, and keeping the temp. at 600-700 deg.C for removing residual carbon to obtain pure A1N whisker. Its advantages are simple process, low cost, and high output rate and quality of said crystal whisker.
Description
The present invention designs a kind of preparation method of aluminium nitride whisker, belongs to technical field of ceramic material.
AlN has high thermal conductivity, superior dielectric properties, piezoelectric property, high surperficial velocity of wave, big advantages such as energy gap, its stupalith become the baseplate material of new generation and the film material with function of hybrid integrated circuit, high density packing material and high-power circuit module.In the research of AlN powder and pottery, it is found that the AlN whisker.Along with the application of increasing crystal whisker materials in matrix material, the AlN whisker is as a kind of novel function whisker, is hopeful enhancing body or the compound crystal whisker materials of function as advanced composite material with its functions peculiar characteristic.The AlN whisker has multiple preparation method, and wherein most typical is distillation coacervation, CVD method and carbothermic method.The distillation coacervation must adopt the AlN powder as raw material, the cost height.In addition, synthetically grown temperature height will strictly be controlled the thermograde of vitellarium, and this has proposed very high requirement to use equipment; The CVD method generally adopts high pure raw material, and it is lower to produce productive rate; Carbothermic method in the past adopts the lower α-Al of price usually
2O
3, graphite is as raw material, is higher than 1700 ℃ but react temperature required, productive rate is low, and morphology is imperfect.
The objective of the invention is to study a kind of preparation method of aluminium nitride whisker, utilize less expensive raw material, by adding suitable mineralizer, in 1550 ℃~1700 ℃ lower wide temperature ranges, carbothermic method obtains AlN whisker high yield, that the whisker structure form is perfect.
The preparation method of the aluminium nitride whisker of the present invention's design is made up of following each step:
1. with α-Al
2O
3Or γ-Al
2O
3Mix mutually with graphite powder or active carbon, its mixed proportion is Al
2O
3: C=1~5: 1, Al
2O
3Granularity be 0.1~100 μ m;
2. above-mentioned compound is mixed mutually with mineralizer, its ratio is:
Compound: 85~100wt%
Mineralizer: 0~10wt%
Mineralizer is Y
2O
3, Dy
2O
3, Ca
2O
3, CaCO
3, CaF
2, Li
2O, B
2O
3Or any in the metallic aluminium powder
One or more mix composition;
3. use ethanol as medium, the powder raw material that above-mentioned second step is prepared mixes with ball mill, and powder raw material is 1: 0.4~0.8 with alcoholic acid composition by weight ratio, and ball milling was laminated or thin stock with dry pressing after 20~30 hours;
4. the base sheet is put into plumbago crucible, in nitrogen flow is 0.5~1.5 liter/minute atmosphere, under 1550~1700 ℃ of temperature, be incubated 1~5 hour, synthetic aluminium nitride whisker;
5. be incubated 2~5 hours down at 600~700 ℃, get rid of residual carbon, promptly get aluminium nitride whisker.
Report about the AlN crystal whisker preparation method all focused on breadboard fundamental research in the past, starting material and use equipment have all been proposed very high requirement, and the actual yield for every kind of method then is not reported, and this makes original AlN Preparation of Whiskers method run into very big obstruction on the road of practicability.And present method makes starting material have alternative within a large range by adopting suitable mineralizer, has reduced the reaction synthesis temperature of whisker; It is synthetic that thin stock that employing dry-pressing or doctor-blade casting process are made or thin slice carry out high temperature.It is simple to have synthesis technique, good reproducibility, high yield, advantages such as low cost.
1. raw-material selectable range is big.Raw-material purity and granularity comprise Al in the method
2O
3, C and mineralizer exert an influence hardly to growth, quality and the productive rate of AlN whisker, this is to be discharged to outside the stove with flowing nitrogen because most impurity and mineralizer mostly form gas phase under the whisker synthesis temperature.Therefore, can adopt in the method inexpensive chemical pure or industrial pure material as the raw material of synthetic AlN whisker, reduce the cost of raw material; Owing to raw-material less demanding, reduced again the requirement to the technical process of synthetic AlN whisker simultaneously, so that this method is easy to grasp and realize in technological operation.
(1) adopts α-Al
2O
3Or γ-Al
2O
3, graphite powder or active carbon be raw material, and purity and the granularity of raw material are not had strict demand.Wherein, α-Al
2O
3Mean particle size at 0.1~100 μ m, the mean particle size of Graphite Powder 99 is at 30~60 μ m; Purity is in 90~100% scopes.
(2) Al in the prescription
2O
3: but the C excursion is big.General Al
2O
3: the excursion of C weight ratio is 1~5: between 1.Select different synthesis temperatures according to different proportionings.
2. the present invention makes the AlN whisker growth initial stage mainly by the growth of VLS mechanism forming core by adding suitable mineralizer.These mineralizers at high temperature are easy to and Al
2O
3Form low-melting compound, thereby provide the liquid growth media for the gas-liquid-solid reaction of AlN whisker.Along with the prolongation of temperature retention time, these low-melting compounds will volatilize gradually, get rid of outside the stove with mobile atmosphere.At later stages, liquid phase is complete obiteration, and active in growth will be helical dislocation mechanism.Therefore, can obtain the AlN whisker of high-purity, structural integrity.
Can adopt Y
2O
3, Dy
2O
3, Ga
2O
3Rare-earth oxide, CaCO
3, CaF
2, Li
2O alkali and alkaline earth metal ions oxide or fluoride, B
2O
3Form as mineralizer Deng one or more mixing in III family oxide and the metallic aluminium powder, addition is between 0~10wt%.
In the method, selected mineralizer has very high unreactiveness to the AlN crystal, with AlN chemical reaction does not take place, and can guarantee the purity and the structural integrity of AlN whisker.
3. be different from other preparation method, present method technology is simple.Whole technical process is similar with the preparation process of conventional pottery.For the requirement of the tight degree of operation then far below the synthesis technique of other whisker.As the degree of uniformity of batch mixing, the quality of pressed compact, the control of synthesis temperature and soaking time etc.This method need not special equipment simultaneously, as long as utilize the equipment of making pottery can reach the equipment requirement of this method
The present invention can select a certain temperature in 1550 ℃~1700 ℃ temperature ranges, be incubated 1~5 hour, synthetic AlN whisker.Technological process is to heating up and the not strict demand of cooling system.
4.AlN whisker is simple with separating of matrix.Under reaction temperature, except major part grew into the AlN whisker, because the existence of liquid phase under the carbon thermal reduction effect, produces the effect of reaction-sintered, base substrate partly became the block of granular AlN after the reaction, and the AlN whisker is very easily separated from base substrate in the base substrate.
Because the above characteristics that the present invention has are compared with AlN crystal whisker preparation method in the past, its technology is simple, and is with low cost; AlN whisker synthetic yield height, quality is good.
Description of drawings:
Fig. 1 is the SEM shape appearance figure of the AlN whisker for preparing of the present invention.
Introduce embodiments of the invention below:
Embodiment 1:
Adopt α-Al
2O
3Powder and graphite powder are as raw material, and the average particle size particle size of two kinds of powder materials is respectively 2.5 and 45 microns, and purity is respectively 99.5 and 98wt%; With B
2O
3And CaF
2As mineralizer.According to percentage by weight α-Al
2O
3: graphite: B
2O
3: CaF
2=68: four kinds of raw materials of weighing in 17: 10: 5.The raw material for preparing is packed in the ball grinder, is to add industrial spirit at 1: 0.5 by the components by weight percent ratio of powder raw material and industrial spirit, dries after 24 hours ball millings mix and sieves, and adopts dry pressing to make the thin stock of φ 20mm * 1mm then.Thin stock is packed in the plumbago crucible, be placed in the graphite atmosphere furnace.Under flowing nitrogen atmosphere, nitrogen flow is 0.5 l/mim, 1650 ℃, and 5 hours synthetic AlN whiskers of constant temperature.At last, synthetic product is placed resistance furnace, under the air atmosphere, 600 ℃, be incubated 4 hours and get rid of remaining C, finally obtain pure AlN whisker.Mol number * 100% of pressing the Al atom in the mol number/raw material of Al atom in whisker productive rate=AlN whisker calculates, and the whisker productive rate of present embodiment is 36%.The whisker that is obtained as shown in Figure 1.
Embodiment 2:
Adopt α-Al
2O
3Powder and graphite powder are as raw material, and the average particle size particle size of two kinds of powder materials is respectively 2.5 and 45 microns, and purity is respectively 99.0 and 97.0wt%; With CaCO
3As mineralizer.According to percentage by weight α-Al
2O
3: graphite: CaCO
3=60: three kinds of raw materials of weighing in 30: 10.The raw material for preparing is packed in the ball grinder, is to add industrial spirit at 1: 0.5 by the components by weight percent ratio of powder raw material and industrial spirit, dries after 24 hours ball millings mix and sieves, and adopts dry pressing to make the thin stock of φ 20mm * 1mm then.Thin stock is packed in the plumbago crucible, be placed in the graphite atmosphere furnace.Under flowing nitrogen atmosphere, nitrogen flow is 0.6 l/mim, 1700 ℃, and 3 hours synthetic AlN whiskers of constant temperature.At last, synthetic product is placed resistance furnace, under the air atmosphere, 600 ℃, be incubated 4 hours and get rid of remaining C, finally obtain the AlN whisker pure, that pattern is perfect, the pattern of whisker is similar to Fig. 1 result.Mol number * 100% of pressing the Al atom in the mol number/raw material of Al atom in whisker productive rate=AlN whisker calculates, and the whisker productive rate that present embodiment obtained is 49%.
Embodiment 3:
Adopt thick emergy and Graphite Powder 99 as raw material, the average particle size particle size of two kinds of powder raw materials is respectively 100 and 45 microns, and purity is respectively 90.0 and 98.0wt%; With CaCO
3As mineralizer.According to the thick emergy of weight percent: graphite: CaCO
3=67.5: three kinds of raw materials of weighing in 22.5: 10.The raw material for preparing is packed in the ball grinder, is to add industrial spirit at 1: 0.5 by the components by weight percent ratio of powder raw material and industrial spirit, dries after 24 hours ball millings mix and sieves, and adopts molded method to make the thin stock of φ 20mm * 1mm then.Thin stock is packed in the plumbago crucible, be placed in the graphite atmosphere furnace.Under flowing nitrogen atmosphere, nitrogen flow is 0.5 l/mim, 1600 ℃, and 5 hours synthetic AlN whiskers of constant temperature.At last, synthetic product is placed resistance furnace, under the air atmosphere, 600 ℃, be incubated 4 hours and get rid of remaining C, finally obtain the AlN whisker pure, that pattern is perfect, the pattern of whisker is similar to Fig. 1 result.Mol number * 100% of pressing the Al atom in the mol number/raw material of Al atom in whisker productive rate=AlN whisker calculates, and the whisker productive rate of present embodiment is 53%.
Embodiment 4:
Adopt γ-Al
2O
3Powder and graphite powder are as raw material, and the average particle size particle size of two kinds of powder materials is respectively 0.04 and 40 micron, and purity is respectively 99.5 and 98.0wt%; With CaCO
3As mineralizer.According to percentage by weight γ-Al
2O
3: graphite: CaCO
3=75: three kinds of raw materials of weighing in 15: 10.The raw material for preparing is packed in the ball grinder, is to add industrial spirit at 1: 0.6 by the components by weight percent ratio of powder raw material and industrial spirit, dries after 24 hours ball millings mix and sieves, and adopts dry pressing to make the thin stock of φ 20mm * 1mm then.Thin stock is packed in the plumbago crucible, be placed in the graphite atmosphere furnace.Under flowing nitrogen atmosphere, nitrogen flow is 0.6 l/mim, 1550 ℃, and 1 hour synthetic AlN whisker of constant temperature.At last, synthetic product is placed resistance furnace, under the air atmosphere, 600 ℃, be incubated 4 hours and get rid of remaining C, finally obtain the AlN whisker pure, that pattern is perfect, the pattern of whisker is similar to Fig. 1 result.Mol number * 100% of pressing the Al atom in the mol number/raw material of Al atom in whisker productive rate=AlN whisker calculates, and the whisker productive rate that present embodiment obtained is 64%.
Claims (1)
1. the preparation method of an aluminium nitride whisker, it is characterized in that this method is made up of following each step: (1) is with α-Al
2O
3Or γ-Al
2O
3Mix mutually with graphite powder or active carbon, its mixed proportion is Al
2O
3: C=1~5: 1, Al
2O
3Granularity be 0.1~100 μ m; (2) above-mentioned compound is mixed mutually with mineralizer, its ratio is:
Compound: 85~100wt%
Mineralizer: 0~10wt%
Mineralizer is Y
2O
3, Dy
2O
3, Ca
2O
3, CaCO
3, CaF
2, Li
2O, B
2O
3Or any in the metallic aluminium powder
One or more mix composition; (3) use ethanol as medium, the powder material that above-mentioned second step is prepared mixes with ball mill, and powder material is 1: 0.4~0.8 with the composition by weight ratio of ethanol, and ball milling was laminated or thin stock with dry pressing after 20~30 hours; (4) the base sheet is put into graphite crucible, in nitrogen flow is 0.5~1.5 liter/min atmosphere, under 1550~1700 ℃ of temperature, be incubated 1~5 hour, synthetic aluminium nitride whisker; (5) 600~700 ℃ of lower insulations 2~5 hours, get rid of residual carbon, namely get aluminium nitride whisker.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN98103409A CN1067969C (en) | 1998-07-24 | 1998-07-24 | Process for preparing aluminium nitride whisker |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN98103409A CN1067969C (en) | 1998-07-24 | 1998-07-24 | Process for preparing aluminium nitride whisker |
Publications (2)
Publication Number | Publication Date |
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CN1203209A true CN1203209A (en) | 1998-12-30 |
CN1067969C CN1067969C (en) | 2001-07-04 |
Family
ID=5217892
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN98103409A Expired - Fee Related CN1067969C (en) | 1998-07-24 | 1998-07-24 | Process for preparing aluminium nitride whisker |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1067969C (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102730730A (en) * | 2012-07-03 | 2012-10-17 | 武汉科技大学 | Submicron Al2O3 fibre and preparation method thereof |
CN104445316A (en) * | 2014-11-07 | 2015-03-25 | 东莞市鸿德电池有限公司 | Preparation method, product and application of nano aluminum oxide material |
CN106699189A (en) * | 2016-11-25 | 2017-05-24 | 河北利福光电技术有限公司 | Aluminum nitride powder for aluminum nitride ceramic substrate and preparation method of aluminum nitride powder |
CN106801258A (en) * | 2016-12-28 | 2017-06-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method with hexa-prism aluminium nitride whisker |
CN107759226A (en) * | 2017-10-29 | 2018-03-06 | 贵州喜文化艺术有限责任公司 | A kind of ceramic powder preparation method |
CN109264678A (en) * | 2018-10-24 | 2019-01-25 | 哈尔滨工业大学(威海) | A kind of preparation method of AlN nano wire |
CN110981523A (en) * | 2019-12-30 | 2020-04-10 | 谢晓佳 | Preparation method of high-strength composite ceramic for circuit board |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2596745B1 (en) * | 1986-04-03 | 1991-06-07 | Atochem | POWDERS FOR CARBIDE AND METAL NITRIDE CERAMICS BY CARBOTHERMAL REDUCTION AND THEIR MANUFACTURING METHOD |
FR2735466B1 (en) * | 1995-06-19 | 1997-08-22 | Aerospatiale | PROCESS FOR PRODUCING ALUMINUM NITRIDE TRICHITES |
US5693305A (en) * | 1995-10-19 | 1997-12-02 | Advanced Refractory Technologies, Inc. | Method for synthesizing aluminum nitride whiskers |
-
1998
- 1998-07-24 CN CN98103409A patent/CN1067969C/en not_active Expired - Fee Related
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102730730A (en) * | 2012-07-03 | 2012-10-17 | 武汉科技大学 | Submicron Al2O3 fibre and preparation method thereof |
CN102730730B (en) * | 2012-07-03 | 2014-06-18 | 武汉科技大学 | Submicron Al2O3 fibre and preparation method thereof |
CN104445316A (en) * | 2014-11-07 | 2015-03-25 | 东莞市鸿德电池有限公司 | Preparation method, product and application of nano aluminum oxide material |
CN104445316B (en) * | 2014-11-07 | 2016-04-13 | 东莞市鸿德电池有限公司 | A kind of preparation method of nano alumina material, goods and application |
CN106699189A (en) * | 2016-11-25 | 2017-05-24 | 河北利福光电技术有限公司 | Aluminum nitride powder for aluminum nitride ceramic substrate and preparation method of aluminum nitride powder |
CN106801258A (en) * | 2016-12-28 | 2017-06-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method with hexa-prism aluminium nitride whisker |
CN107759226A (en) * | 2017-10-29 | 2018-03-06 | 贵州喜文化艺术有限责任公司 | A kind of ceramic powder preparation method |
CN109264678A (en) * | 2018-10-24 | 2019-01-25 | 哈尔滨工业大学(威海) | A kind of preparation method of AlN nano wire |
CN110981523A (en) * | 2019-12-30 | 2020-04-10 | 谢晓佳 | Preparation method of high-strength composite ceramic for circuit board |
Also Published As
Publication number | Publication date |
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CN1067969C (en) | 2001-07-04 |
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