CN104658624B - Radiation shielding electronic packaging material and preparation method for same - Google Patents
Radiation shielding electronic packaging material and preparation method for same Download PDFInfo
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- CN104658624B CN104658624B CN201510039799.XA CN201510039799A CN104658624B CN 104658624 B CN104658624 B CN 104658624B CN 201510039799 A CN201510039799 A CN 201510039799A CN 104658624 B CN104658624 B CN 104658624B
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Abstract
The invention discloses a radiation shielding electronic packaging material, which comprises a sintered body of a composition, wherein the composition comprises heavy metal or heavy metal compound powder serving as a radiation shielding functional component, alumina ceramic powder serving as a substrate component, a sintering aid and an adhesive. The radiation shielding electronic packaging material is prepared by the following steps: uniformly mixing the heavy metal or heavy metal compound powder, the alumina ceramic powder and the sintering aid by taking an organic solvent as a dispersion medium; mixing the adhesive into the mixture after the mixture is dried, and performing granulation to obtain composite granules; performing dry-pressing molding and high-temperature sintering. The obtained material has high ray shielding performance, particularly high X and gamma ray radiation shielding performance.
Description
Technical field
The invention belongs to electronic package material field, and in particular to the electronics with high energy X, gamma Rays barrier propterty
Encapsulating material and preparation method thereof.
Background technology
The electronic component worked in high-energy particle radiation environment, due to the radiation hardness grade of electronic device and chip it is very low, especially
Chip etc. by after X, gamma Rays, radiating particle by with material in electron interaction, produce ionisation effect and
Chip is damaged, the performance degradation of integrated circuit is caused, causes the even completely permanent damage of logic function mistake, so as to cause electricity
Subcomponent global failure.Radiation shield can effectively improve the radiation hardness grade of electronic device and chip.But existing screen method
Exist single, thick and heavy shielding material, processing difficulties, it is poisonous the shortcomings of.
Electronic package material is with plastics, ceramic main at present.Wherein plastics radiation resistance is poor, heavy dose of rate ray spoke
The reactions such as aging, degraded are susceptible to according under, and thermal coefficient of expansion is big, it is poor with chip matching.Ceramics itself have resistance to
Radiance is good, mechanical strength is high, chemical resistance and the low advantage of thermal coefficient of expansion, is a kind of excellent Electronic Packaging
Material.But ceramics hardly have radiation shield performance, need to be modified which so as to effectively improve encapsulating material to core
The radiation protection performance of piece.
The Chinese patent of Publication No. CN102424568A discloses a kind of preparation of tungsten-containing alumina ceramic heating substrate
Method, the method are prepared for aluminium oxide ceramic chips using aqueous tape casting forming technique, and organizine net is printed on aluminium oxide ceramic chips surface
Uniform deposition tungsten is starched, then obtains tungstenic aluminium oxide heating base plate through sintering, nickel plating technology.Ceramic heating base prepared by the invention
Plate quality is good, high yield rate, low production cost.But the content of tungsten is relatively low, heating base plate material is used only as.
The Chinese patent of Publication No. CN101569929A discloses a kind of preparation method of nano aluminum oxide coated tungsten powder,
Belong to field of powder metallurgy preparation, ammonium metawolframate powder and Aluminium Sulphate usp (powder) are codissolved in distilled water by being mainly characterized by of the method
In, pre-freeze in liquid nitrogen being dispersed in, is vacuum dried, Jing hydrogen reducings obtain the composite granule of nano aluminum oxide coated tungsten powder, effectively
The problems such as solving irregular nano aluminum oxide coated tungsten powder granularity, powder reuniting.But the method complex forming technology, cost compared with
High, yield is relatively low, it is difficult to which large-scale promotion is used.
The content of the invention
It is an object of the invention to provide one kind has preferable shielding propertiess for X, gamma-rays, and bi-material can be passed through
It is compound to realize high-termal conductivity and low thermal expansion simultaneously, so as to obtaining the radiation shield electronic package material of excellent combination property and being somebody's turn to do
The preparation method of material.
First aspect present invention is a kind of radiation shield electronic package material, and which includes the sintered body of compositionss, described group
Compound includes：Heavy metal or its compound powder as radiation shield function ingredients；As the alumina ceramics powder of matrix component
Body；Sintering aid；And binding agent.
According to the radiation shield electronic package material of preferred embodiment, wherein heavy metal or its compound in the compositionss
Powder body, alumina ceramics powder body, sintering aid content be respectively 10.0wt%～90.0wt%, 10.0wt%～88.0wt%,
1.0wt%～8.2wt%；And the addition of binding agent is 0.5wt%～10.0wt%.
According to the radiation shield electronic package material of preferred embodiment, wherein heavy metal or its compound powder be tungsten, tantalum,
One or more in lead, bismuth, barium, tungsten oxide, tantalum pentoxide, lead oxide, bismuth oxide, Barium monoxide, tungsten carbide；Alumina powder
Body is 90 porcelain powder, 95 porcelain powder, one or more in 99 porcelain powder；Sintering aid is silicon dioxide, magnesium oxide, calcium oxide, oxidation
One or more in yttrium, lanthana；And the binding agent is that concentration is the polyvinyl alcohol of 3.0wt%～12.0wt%, epoxy
The aqueous solution of resin or phenolic resin.
The present invention also provides a kind of method for preparing preceding claim radiation shield electronic package material, including following step
Suddenly：Heavy metal or its compound powder, alumina ceramics powder body and sintering aid are with organic solvent as disperse medium mix homogeneously；It is dry
Binding agent is mixed into after dry, pelletize obtains composite particles；And dry-pressing formed rear high temperature sintering.
The present invention also provides purposes of the described radiation shield electronic package material in shielding X, gamma Rays.
The heavy metal prepared using said method or the porosity of its compound/alumina composite encapsulating material are less, heat
The coefficient of expansion is relatively low, and heat conductivility is preferable.It is using Co-60 as irradiation bomb, multiple to gained heavy metal or its compound/alumina
The radiation shield performance for closing encapsulating material carries out shielding propertiess test.Composite encapsulating material has good alpha ray shield performance.
Description of the drawings
Fig. 1 is the preparation flow figure of heavy metal or its compound/alumina composite encapsulating material.
Metallurgical microscope figures of the Fig. 2 for 1 gained composite encapsulating material of embodiment.
Scanning electron microscope (SEM) photographs of the Fig. 3 for 1 gained composite encapsulating material section of embodiment.
X-ray diffractograms of the Fig. 4 for 1 gained composite encapsulating material of embodiment.
Specific embodiment
The present invention is comprised the following steps：
(1) by heavy metal or its compound (preferably oxide or carbide), alumina powder jointed, sintering aid, to have
Machine solvent is used as disperse medium, mix homogeneously.It is dried to obtain heavy metal or its compound/alumina composite powder.
(2) binding agent is added to heavy metal or its compound/alumina composite powder, mixing granulation.
(3) will be the heavy metal for obtaining or its compound/alumina composite particles dry-pressing formed, obtain heavy metal or its chemical combination
Thing/alumina composite material green compact.
(4) green compact for obtaining are dried, after be placed in high temperature process furnances high temperature sintering, obtain heavy metal or its compound/
Alumina composite encapsulating material.
Heavy metal or its compound described in step (1) be tungsten, tantalum, lead, bismuth, barium, tungsten oxide, tantalum pentoxide,
One or more in lead oxide, bismuth oxide, Barium monoxide, tungsten carbide, its addition are 10.0wt%～90.0wt%.Described
It is alumina powder jointed be 90 porcelain powder, 95 porcelain powder, one or more in 99 porcelain powder, its addition is 10.0wt%～88.0wt%.
Described sintering aid is silicon dioxide, magnesium oxide, calcium oxide, yittrium oxide, one or more in lanthana, and its addition is
1.0wt%～8.2wt%.Described disperse medium can be one or more in methanol, ethanol, isopropanol, acetone, toluene.
In step (2), the binding agent is poly-vinyl alcohol solution, epoxy resin solution, in phenol resin solution one
Kind, the agglomerant concentration is 3.0wt%～12.0wt%, and addition is 0.5wt%～10.0wt%.
In step (4), sintering temperature is 1250～1750 DEG C, 100～300min of temperature retention time under maximum temperature.
Embodiment 1
Composite powder is consisted of：Tungsten powder 14g, 95 alumina ceramics powder 25g, silicon dioxide 2.0g；Ethanol is situated between as dispersion
Matter, mix homogeneously.Add the 7.0wt% phenol resin solutions of 1.1g as binding agent after drying, mixing granulation obtains tungsten/oxidation
Aluminum composite particles.Sinter tungsten/alumina composite granule dry-pressing formed after high temperature process furnances high temperature, sintering temperature is 1400
DEG C, 200min is incubated, tungsten/alumina composite encapsulating material is obtained.
Fig. 2, Fig. 3 and Fig. 4 respectively illustrate the metallurgical microscope figure of gained composite encapsulating material, the scanning electricity of material section
Mirror figure, the X-ray diffractogram of material.
Embodiment 2
Composite powder is consisted of：Tantalum powder 63g, 95 alumina ceramics powder 30g, silicon dioxide 0.5g, yittrium oxide 1.1g；Methanol
As disperse medium, mix homogeneously.The 9.0wt% poly-vinyl alcohol solutions of 1.2g are added after drying as binding agent, mixing granulation
Obtain tantalum/alumina composite granule.Sinter tantalum/alumina composite granule dry-pressing formed after high temperature process furnances high temperature, burn
Junction temperature is 1400 DEG C, is incubated 100min, obtains tantalum/alumina composite encapsulating material.
Embodiment 3
Composite powder is consisted of：Bismuth oxide powder 30g, 95 alumina ceramics powder 15g, calcium oxide 0.8g, silicon dioxide
0.8g；Acetone is used as disperse medium, mix homogeneously.The 4.0wt% poly-vinyl alcohol solutions of 2.8g are added after drying as binding agent,
Mixing granulation obtains bismuth oxide/alumina composite granule.Will be bismuth oxide/alumina composite granule dry-pressing formed after high-temperature tubular
Stove high temperature is sintered, and sintering temperature is 1500 DEG C, is incubated 200min, obtains bismuth oxide/alumina composite encapsulating material.
Embodiment 4
Composite powder is consisted of：Tungsten oxide powder body 44g, 90 alumina ceramics powder 21g, magnesium oxide 2.0g；Isopropanol conduct
Disperse medium, mix homogeneously add the 10.0wt% epoxy resin solutions of 1.2g as binding agent after being dried, mixing granulation is obtained
Tungsten oxide/alumina composite granule.Burn tungsten oxide/alumina composite granule dry-pressing formed after high temperature process furnances high temperature
Knot, sintering temperature are 1450 DEG C, are incubated 150min, obtain tungsten oxide/alumina composite encapsulating material.
Embodiment 5
Composite powder is consisted of：Barium monoxide powder body 35g, 95 alumina ceramics powder 26g, magnesium oxide 2.0g, titanium dioxide lanthanum
0.6g；Ethanol adds the 10.0wt% epoxy resin solutions of 1.2g as bonding as disperse medium, mix homogeneously after being dried
Agent, mixing granulation obtain Barium monoxide/alumina composite granule.Will be Barium monoxide/alumina composite granule dry-pressing formed after high temperature
Tube furnace high temperature is sintered, and sintering temperature is 1350 DEG C, is incubated 220min, obtains Barium monoxide/alumina composite encapsulating material.
Embodiment 6
Composite powder is consisted of：Bismuth meal 6.2g, 95 alumina ceramics powder 50g, silicon dioxide 3.0g；Methanol is situated between as dispersion
Matter, mix homogeneously.Add the 7.0wt% poly-vinyl alcohol solutions of 1.1g as binding agent after drying, mixing granulation obtains bismuth/oxidation
Aluminum composite particles.Sinter bismuth/alumina composite granule dry-pressing formed after high temperature process furnances high temperature, sintering temperature is 1550
DEG C, 250min is incubated, bismuth/alumina composite encapsulating material is obtained.
Embodiment 7
Composite powder is consisted of：Tungsten carbide 110g, 95 alumina ceramics powder 25g, magnesium oxide 2.0g；Ethanol is situated between as dispersion
Matter, mix homogeneously.After drying add 1.4g 7.0wt% poly-vinyl alcohol solutions as binding agent, mixing granulation obtain tungsten carbide/
Alumina composite granule.Sinter tungsten carbide/alumina composite granule dry-pressing formed after high temperature process furnances high temperature, sintering temperature
Spend for 1750 DEG C, be incubated 200min, obtain tungsten carbide/alumina composite encapsulating material.
With Co-60 radioactive sources as irradiation bomb, the shielding propertiess of composite are tested.Test result such as following table institute
Show：
Comparative example
The performance data of the radiation shield of the electron device package material being most frequently with present is given below.Using casting method
The screen of the epoxy resin encapsulating material (comparative example 1) of preparation and the aluminium oxide ceramics (comparative example 2) prepared using dry pressing
Cover performance as shown in the table：
By comparing, prepared radiation shield electronic package material radiation shield performance is significantly improved.
Claims (3)
1. a kind of radiation shield electronic package material, the radiation shield electronic package material is by the following preparation side of key step
Method is obtained：
Heavy metal or its compound powder, alumina ceramics powder body and sintering aid are with organic solvent as disperse medium mix homogeneously；
Binding agent is mixed into after drying, pelletize obtains composite particles；And
Above-mentioned composite particles are obtained into object Jing after dry-pressing formed and sintering；
Wherein, the heavy metal or its compound powder, alumina ceramics powder body, the content of sintering aid be respectively 10.0wt%～
90.0wt%, 10.0wt%～88.0wt%, 1.0wt%～8.2wt%, the addition of binding agent be 0.5wt%～
10.0wt%；
The sintering temperature is 1250 DEG C～1750 DEG C, temperature retention time 100min～300min；
The heavy metal or its compound powder are selected from：Tungsten, tantalum, lead, bismuth, barium, tungsten oxide, tantalum pentoxide, lead oxide, oxidation
In bismuth, Barium monoxide or tungsten carbide one or more；
The alumina ceramics powder body is selected from：In 90 porcelain powder, 95 porcelain powder or 99 porcelain powder one or more；
The sintering aid is selected from：In silicon dioxide, magnesium oxide, calcium oxide, yittrium oxide or lanthana one or more；
The binding agent is the aqueous solution of the polyvinyl alcohol that concentration is 3.0wt%～12.0wt%, epoxy resin or phenolic resin；
The maskable X of gained object, gamma Rays.
2. radiation shield electronic package material as claimed in claim 1, it is characterised in that wherein heavy metal or its compound powder
Body, alumina ceramics powder body, the content of sintering aid are respectively 10.0wt%～80.0wt%, 18.2wt%～81.8wt%,
1.0wt%～8.2wt%.
3. radiation shield electronic package material as claimed in claim 1 or 2, it is characterised in that organic solvent choosing wherein used
From：In methanol, ethanol, isopropanol, acetone or toluene one or more.
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| CN105647122B (en) * | 2016-03-22 | 2018-02-27 | 林飘飘 | A kind of radiation shield composite and preparation method thereof |
| CN106811662A (en) * | 2016-12-30 | 2017-06-09 | 东莞市佳乾新材料科技有限公司 | A kind of preparation method of the electronic package material with radiation-resisting functional |
| CN111403063B (en) * | 2018-12-13 | 2023-11-10 | 苏州嘉乐威新材料股份有限公司 | Radiation protection composition, radiation protection material and radiation protection product |
| CN112071459A (en) * | 2020-09-07 | 2020-12-11 | 圣华盾防护科技股份有限公司 | X/gamma ray shielding composite material based on polyvinyl alcohol through-hole foam and preparation method thereof |
| CN112599271A (en) * | 2020-12-14 | 2021-04-02 | 有研工程技术研究院有限公司 | Electron radiation resistant multilayer structure shielding material and preparation method thereof |
| CN113683909B (en) * | 2021-09-02 | 2022-07-12 | 上海大学 | Nano bismuth oxide anti-radiation ceramic coating, preparation method and application |
| CN115376716B (en) * | 2022-08-11 | 2023-06-16 | 哈尔滨工业大学 | High-entropy ceramic oxide coating for shielding neutrons and gamma rays and preparation method thereof |
| CN115799227B (en) * | 2023-01-10 | 2023-06-09 | 荣耀终端有限公司 | Bare chip, chip and electronic device |
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| JPS6442359A (en) * | 1987-08-11 | 1989-02-14 | Narumi China Corp | Black alumina ceramic composition |
| US5112697A (en) * | 1989-09-06 | 1992-05-12 | Alcan International Limited | Stabilized metal foam body |
| KR100215485B1 (en) * | 1996-09-19 | 1999-08-16 | 나창호 | Ceramic composition and method thereof |
| JP2004349476A (en) * | 2003-05-22 | 2004-12-09 | Toshiba Corp | Semiconductor device |
| CN101472841B (en) * | 2006-05-12 | 2012-05-02 | 电气化学工业株式会社 | Ceramic powder and method of using the same |
| JP5680187B2 (en) * | 2011-03-30 | 2015-03-04 | サン−ゴバン セラミックス アンド プラスティクス，インコーポレイティド | Refractories, glass overflow molding blocks and methods and uses of refractories |
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