CN103101915A - Preparation method of fused silica powder for electronic integrated circuit package - Google Patents

Preparation method of fused silica powder for electronic integrated circuit package Download PDF

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CN103101915A
CN103101915A CN 201210069134 CN201210069134A CN103101915A CN 103101915 A CN103101915 A CN 103101915A CN 201210069134 CN201210069134 CN 201210069134 CN 201210069134 A CN201210069134 A CN 201210069134A CN 103101915 A CN103101915 A CN 103101915A
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quartz
integrated circuit
electronic integrated
granularity
sent
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CN 201210069134
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张雷
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Jiangsu Ronghui Quartz Material Scitech Co Ltd
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Jiangsu Ronghui Quartz Material Scitech Co Ltd
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Abstract

The invention discloses a preparation method of fused silica powder for electronic integrated circuit package. The product belongs to the field of finish machining of quartz stone. The method uses high-purity quartz stone as a raw material, and a series of processes of crushing, scouring, water purifying, high-temperature sintering, crushing, magnetically separating, grinding, and magnetically separating are performed, wherein the process flow has the advantages of less device investment, low production cost, and no sewage and waste gas discharge, the fused silica powder for electronic integrated circuit package with high quality can be produced in batches; the product has a series of advantages of high temperature resistance, low-heat expansion, high hardness, good abrasion resistance, excellent transmitting refraction and piezoelectric property, and is the first choice for electronic integrated circuit package.

Description

A kind of electronic integrated circuit encapsulation preparation method of molten silicon micro mist
Technical field
The invention belongs to quartzite precision work field, relate in particular to a kind of take high grade quartz stone as primary industry production electronic integrated circuit encapsulation with the method for molten silicon micro mist.
Background technology
integrated antenna package is through melting take high grade quartz stone as raw material with the molten silicon micro mist, the series of process such as grinding processing and a kind of product of making, the content of its silicon-dioxide is not less than 99.8%, during production with the melting in electric arc furnace or resistance furnace or high temperature sintering furnace of selected high grade quartz stone, melt temperature is 1800 ℃-1900 ℃, become molten state after melting 11-15 hour, become the solid fused quartz after cooling, because its atomic structure long-range is unordered, its three-dimensional structure is cross-linked makes it have resistance to elevated temperatures strong (fusing point is 1730 ℃), thermal expansivity is low, hardness higher (Mohs' hardness is 7), wear resisting property is good, printing opacity refraction performance, piezoelectric property is excellent, under normal temperature not with the advantages such as each substance reaction, thereby of many uses, can be used as refractory materials, ceramic raw material, poured with epoxy resin, the electronic integrated circuit encapsulation, electric light source, medical treatment, casting, the raw material of the industries such as photovoltaic.The present invention is a kind of electronic integrated circuit package specific molten silicon micro mist; the electronic integrated circuit encapsulation refers to the circuit pin on silicon chip; connect with wire and guide to external lug place; in order to be connected with other device; it not only plays a part to install, fixes, seals, protects the aspects such as chip and enhancing electric heating property; but also be wired to by the contact on chip on the pin of package casing; these pins are connected with other devices by the wire on printed circuit board (PCB) again, thereby realize being connected of inside chip and external circuit.Electronic integrated circuit encapsulation is in playing integrated circuit (IC) chip bonding point and the outside effect that is electrically connected; also provide a reliable and stable Working environment for integrated circuit (IC) chip; integrated circuit (IC) chip is played machinery or Environmental Role; thereby integrated circuit (IC) chip can be worked, and guarantee that it has high stability and reliability.The quality of integrated antenna package quality, very large to the good and bad relation of the overall performance of unicircuit, therefore, packaged material should have stronger mechanical property, good electric property, heat dispersion and chemical stability.Due to the requirement of unicircuit and the difference of field of employment, can select different packaged materials, these materials have: 1. the mixture of organic resin and wax encapsulation, shortcoming is poor reliability; 2. rubber packaging, it is heat-resisting, oil resistant and electrical property undesirable; 3. plastic pattern encapsulation, shortcoming are that thermotolerance is relatively poor and have a water absorbability; 4. molten silicon micro mist-Metal Packaging, because the molten silicon micro mist has high temperature resistant, low thermal coefficient of expansion, under normal temperature not with each substance reaction, hardness is higher, wear resistance good, the series of advantages such as printing opacity refraction performance, piezoelectric property excellence, can overcome first three and plant the defective that material has, make it become a kind of electronic integrated circuit packaged material of excellent property.The difference that encapsulation requires according to electronic integrated circuit, the molten silicon micro powder granule degree of use is generally the 300-3000 order.Product of the present invention be a kind of specification be 300-3000 purpose electronic integrated circuits encapsulation to use molten silicon micro mist, outward appearance be white powder, SiO2 content is more than 99.8%.Produce this product take high grade quartz stone as raw material, take high temperature sintering furnace and grinding machinery as major equipment, the series of process such as, high temperature sintering pure by fragmentation, pickling, water extraction to high grade quartz stone, fragmentation, magnetic separation, grinding, magnetic separation process, the major advantage of this technical process is: facility investment is few, production cost is low, without the sewage exhaust gas emission, can be mass, can produce high-quality electronic integrated circuit encapsulation molten silicon micro mist.
Summary of the invention
Very poor for the mixture packaged material reliability that overcomes organic resin and wax, the rubber packaging material is heat-resisting, oil resistant and electrical property is undesirable, plastic pattern material package thermotolerance is relatively poor and have hygroscopic defective, the invention provides a kind of electronic integrated circuit packaged material of excellent performance-molten silicon micro mist, the series of advantages such as that this material has is high temperature resistant, low thermal coefficient of expansion, hardness is higher, wear resistance good, piezoelectric property is excellent become the first-selection of electronic integrated circuit packaged material.Producing the raw material that this product uses has: high grade quartz stone, concentration are the dilute hydrochloric acid of 10%-15%, concentration hydrofluoric acid, the water as 45%-47%.
The present invention can be achieved through the following technical solutions:
A kind of electronic integrated circuit encapsulation production method of molten silicon micro mist is characterized in that being made of following steps:
(1) quartzite of high-quality bulk is sent into rinsing machine, use high pressure water washing, remove dirt settling, it is that granularity is the quartz wedge of 2mm-20mm that the boulder diamond stone after then washing is sent into crusher in crushing.
(2) quartz wedge after fragmentation is sent into sour pond, be that the mixing acid that the dilute hydrochloric acid of 10%-15% and hydrofluoric acid that concentration is 45%-47% mix in the ratio of 3:1 soaked 75-80 hour with concentration, the purpose of pickling is to remove dirt settling contained in quartz sand and metal oxide.
(3) with after the quartz wedge deacidification after the mixing acid immersion, send into immediately the rinsing machine water and rinse, the quartz wedge of cleaning is sent into high temperature sintering furnace after screening, feeding temperature-raising, transferring the interior temperature of stove is 1800 ℃-1900 ℃, and fusing time is 11-15 hour, makes the interior quartzite of stove become molten state.
(4) fusing stops powering to high temperature sintering furnace after finishing, be cooled to the solid fused quartz that normal temperature obtains bulk after cooling, sorting obtains the quartz particles of 5mm-10mm after mechanical or artificial method fragmentation, send into magnetic separator with the quartz particles that is about to 5mm-10mm and carry out magnetic separation, the magnetic separation time is 0.2-0.3 hour, will contain magnetic, the removal of metallic quartz particles.
(5) quartz particles after magnetic separation being put into shredder grinds, input speed and the discharging speed of controlling shredder are balanced, for the 1.4-1.5 ton/hour, the rotating speed of shredder is 23-25 rev/min, milling time is controlled to be 128-700 minute, and the powder after grinding is delivered to grading machine through induced draft fan wind, and granularity continues to grind greater than the shredder that returns of 300 order silicon powders, granularity is that 300-3000 order silicon powder enters collector, and granularity reserves for other use after packing less than 3000 purpose silicon powders.
(6) be that 300-3000 purpose molten silicon micro mist is sent into magnetic separator with granularity in collector, to contain magnetic and metallic silicon powder removes, the magnetic separation time is 0.3-0.5 hour, obtain electronic integrated circuit package specific molten silicon micro mist after magnetic separation, the content of its silicon-dioxide obtains finished product more than 99.8% after packing.
In above-mentioned steps (2), the leaching time of quartzite is 75; 77.5; 80 hours.
When the melt temperature in above-mentioned steps (3) is 1800 ℃, corresponding fusing time is 15 hours; When melt temperature is 1850 ℃, corresponding fusing time is 13 hours; When melt temperature is 1900 ℃, corresponding fusing time is 11 hours.
The invention has the beneficial effects as follows: the production method of a kind of electronic integrated circuit encapsulation with the molten silicon micro mist is provided, this production method has: facility investment is few, production cost is low, without the sewage exhaust gas emission, can be mass out high-quality electronic integrated circuit encapsulation molten silicon micro mist, the series of advantages such as that product has is high temperature resistant, low-thermal-expansion, hardness is higher, wear resistance good, printing opacity refraction performance, piezoelectric property excellence are the preferred material that the electronic integrated circuit encapsulation is used.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The quartzite of high-quality bulk is sent into rinsing machine, use high pressure water washing, remove dirt settling, it is that granularity is the quartz wedge of 2mm-20mm that the boulder diamond stone after then washing is sent into crusher in crushing; Quartz wedge after fragmentation is sent into sour pond, is that 10% dilute hydrochloric acid and concentration are that the mixing acid that 47% hydrofluoric acid mixes in the ratio of 3:1 soaked 75 hours with concentration, and the purpose of pickling is to remove dirt settling contained in quartz sand and metal oxide; After quartz wedge after mixing acid is soaked deacidifies, send into immediately the flushing of rinsing machine water, the quartz wedge of cleaning is sent into high temperature sintering furnace after screening, feeding temperature-raising, and transferring the interior temperature of stove is 1800 ℃, fusing time is 15 hours, makes the interior quartzite of stove become molten state; Fusing stops powering to high temperature sintering furnace after finishing, be cooled to the solid fused quartz that normal temperature obtains bulk after cooling, sorting obtains the quartz particles of 5mm-10mm after mechanical or artificial method fragmentation, send into magnetic separator with the quartz particles that is about to 5mm-10mm and carry out magnetic separation, the magnetic separation time is 0.2 hour, will contain magnetic, the removal of metallic quartz particles; Quartz particles after magnetic separation is put into shredder to be ground, input speed and the discharging speed of controlling shredder are balanced, for the 1.4-1.5 ton/hour, the rotating speed of shredder is 23 rev/mins, milling time is controlled to be 128-700 minute, and the powder after grinding is delivered to grading machine through induced draft fan wind, and granularity continues to grind greater than the shredder that returns of 300 order silicon powders, granularity is that 300-3000 order silicon powder enters collector, and granularity reserves for other use after packing less than 3000 purpose silicon powders; Be that 300-3000 purpose molten silicon micro mist is sent into magnetic separator with granularity in collector, to contain magnetic and metallic silicon powder removes, the magnetic separation time is 0.5 hour, obtain electronic integrated circuit package specific molten silicon micro mist after magnetic separation, the content of its silicon-dioxide obtains finished product more than 99.8% after packing.
Embodiment 2
The quartzite of high-quality bulk is sent into rinsing machine, use high pressure water washing, remove dirt settling, it is that granularity is the quartz wedge of 2mm-20mm that the boulder diamond stone after then washing is sent into crusher in crushing; Quartz wedge after fragmentation is sent into sour pond, is that 12.5% dilute hydrochloric acid and concentration are that the mixing acid that 46% hydrofluoric acid mixes in the ratio of 3:1 soaked 77.5 hours with concentration, and the purpose of pickling is to remove dirt settling contained in quartz sand and metal oxide; After quartz wedge after mixing acid is soaked deacidifies, send into immediately the flushing of rinsing machine water, the quartz wedge of cleaning is sent into high temperature sintering furnace after screening, feeding temperature-raising, and transferring the interior temperature of stove is 1850 ℃, fusing time is 13 hours, makes the interior quartzite of stove become molten state; Fusing stops powering to high temperature sintering furnace after finishing, be cooled to the solid fused quartz that normal temperature obtains bulk after cooling, sorting obtains the quartz particles of 5mm-10mm after mechanical or artificial method fragmentation, send into magnetic separator with the quartz particles that is about to 5mm-10mm and carry out magnetic separation, the magnetic separation time is 0.25 hour, will contain magnetic, the removal of metallic quartz particles; Quartz particles after magnetic separation is put into shredder to be ground, input speed and the discharging speed of controlling shredder are balanced, for the 1.4-1.5 ton/hour, the rotating speed of shredder is 24 rev/mins, milling time is controlled to be 128-700 minute, and the powder after grinding is delivered to grading machine through induced draft fan wind, and granularity continues to grind greater than the shredder that returns of 300 order silicon powders, granularity is that 300-3000 order silicon powder enters collector, and granularity reserves for other use after packing less than 3000 purpose silicon powders; Be that 300-3000 purpose molten silicon micro mist is sent into magnetic separator with granularity in collector, to contain magnetic and metallic silicon powder removes, the magnetic separation time is 0.4 hour, obtain electronic integrated circuit package specific molten silicon micro mist after magnetic separation, the content of its silicon-dioxide obtains finished product more than 99.8% after packing.
Embodiment 3
The quartzite of high-quality bulk is sent into rinsing machine, use high pressure water washing, remove dirt settling, it is that granularity is the quartz wedge of 2mm-20mm that the boulder diamond stone after then washing is sent into crusher in crushing; Quartz wedge after fragmentation is sent into sour pond, is that 15% dilute hydrochloric acid and concentration are that the mixing acid that 45% hydrofluoric acid mixes in the ratio of 3:1 soaked 80 hours with concentration, and the purpose of pickling is to remove dirt settling contained in quartz sand and metal oxide; After quartz wedge after mixing acid is soaked deacidifies, send into immediately the flushing of rinsing machine water, the quartz wedge of cleaning is sent into high temperature sintering furnace after screening, feeding temperature-raising, and transferring the interior temperature of stove is 1900 ℃, fusing time is 11 hours, makes the interior quartzite of stove become molten state; Fusing stops powering to high temperature sintering furnace after finishing, be cooled to the solid fused quartz that normal temperature obtains bulk after cooling, sorting obtains the quartz particles of 5mm-10mm after mechanical or artificial method fragmentation, send into magnetic separator with the quartz particles that is about to 5mm-10mm and carry out magnetic separation, the magnetic separation time is 0.3 hour, will contain magnetic, the removal of metallic quartz particles; Quartz particles after magnetic separation is put into shredder to be ground, input speed and the discharging speed of controlling shredder are balanced, for the 1.4-1.5 ton/hour, the rotating speed of shredder is 25 rev/mins, milling time is controlled to be 128-700 minute, and the powder after grinding is delivered to grading machine through induced draft fan wind, and granularity continues to grind greater than the shredder that returns of 300 order silicon powders, granularity is that 300-3000 order silicon powder enters collector, and granularity reserves for other use after packing less than 3000 purpose silicon powders; Be that 300-3000 purpose molten silicon micro mist is sent into magnetic separator with granularity in collector, to contain magnetic and metallic silicon powder removes, the magnetic separation time is 0.3-hour, obtain electronic integrated circuit package specific molten silicon micro mist after magnetic separation, the content of its silicon-dioxide obtains finished product more than 99.8% after packing.

Claims (3)

1. electronic integrated circuit encapsulation is with the preparation method of molten silicon micro mist, and the raw material that uses is the dilute hydrochloric acid of 10%-15%, concentration hydrofluoric acid, the water as 45%-47% as high grade quartz stone, concentration; It is characterized in that: step (1) is sent the quartzite of high-quality bulk into rinsing machine, uses high pressure water washing, removes dirt settling, and it is that granularity is the quartz wedge of 2mm-20mm that the boulder diamond stone after then washing is sent into crusher in crushing; Step (2) is sent the quartz wedge after fragmentation into sour pond, be that the mixing acid that the dilute hydrochloric acid of 10%-15% and hydrofluoric acid that concentration is 45%-47% mix in the ratio of 3:1 soaked 75-80 hour with concentration, the purpose of pickling is to remove dirt settling contained in quartz sand and metal oxide; After quartz wedge deacidification after step (3) is soaked mixing acid, send into immediately the rinsing machine water and rinse, the quartz wedge of cleaning is sent into high temperature sintering furnace after screening, feeding temperature-raising, transferring the interior temperature of stove is 1800 ℃-1900 ℃, and fusing time is 11-15 hour, makes the interior quartzite of stove become molten state; After finishing, step (4) fusing stops powering to high temperature sintering furnace, be cooled to the solid fused quartz that normal temperature obtains bulk after cooling, sorting obtains the quartz particles of 5mm-10mm after mechanical or artificial method fragmentation, send into magnetic separator with the quartz particles that is about to 5mm-10mm and carry out magnetic separation, the magnetic separation time is 0.2-0.3 hour, will contain magnetic, the removal of metallic quartz particles; Step (5) is put into shredder with quartz particles after magnetic separation and is ground, input speed and the discharging speed of controlling shredder are balanced, for the 1.4-1.5 ton/hour, the rotating speed of shredder is 23-25 rev/min, milling time is controlled to be 128-700 minute, powder after grinding is delivered to grading machine through induced draft fan wind, granularity continues to grind greater than the shredder that returns of 300 order silicon powders, granularity is that 300-3000 order silicon powder enters collector, and granularity reserves for other use after packing less than 3000 purpose silicon powders; Step (6) is that 300-3000 purpose molten silicon micro mist is sent into magnetic separator with granularity in collector, to contain magnetic and metallic silicon powder removes, the magnetic separation time is 0.3-0.5 hour, obtain electronic integrated circuit package specific molten silicon micro mist after magnetic separation, the content of its silicon-dioxide obtains finished product more than 99.8% after packing.
2. a kind of electronic integrated circuit according to claim 1 encapsulates the preparation method with the molten silicon micro mist, and the feature of its step (2) is: the leaching time of described quartzite is 75; 77.5; 80 hours.
3. a kind of electronic integrated circuit encapsulation according to claim 1 is with the preparation method of molten silicon micro mist, and the feature of its step (3) is: when described melt temperature is 1800 ℃, corresponding fusing time is 15 hours; When melt temperature is 1850 ℃, corresponding fusing time is 13 hours; When melt temperature is 1900 ℃, corresponding fusing time is 11 hours.
CN 201210069134 2012-03-16 2012-03-16 Preparation method of fused silica powder for electronic integrated circuit package Pending CN103101915A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663472A (en) * 2013-11-21 2014-03-26 成都兴能新材料有限公司 Preparation method for fused fine silicon powder
CN105084373A (en) * 2015-07-24 2015-11-25 陈林 Method for preparing low-dielectric-constant silica powder
CN106315591A (en) * 2016-08-25 2017-01-11 仇颖超 Method for preparing high-purity fused silica micropowder by composite plant acid
CN113798037A (en) * 2021-09-13 2021-12-17 苏州锐朗新材料有限公司 Raw material pretreatment process suitable for chip packaging materials with different attributes

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663472A (en) * 2013-11-21 2014-03-26 成都兴能新材料有限公司 Preparation method for fused fine silicon powder
CN103663472B (en) * 2013-11-21 2015-12-09 成都兴能新材料有限公司 A kind of preparation method of molten silicon micro mist
CN105084373A (en) * 2015-07-24 2015-11-25 陈林 Method for preparing low-dielectric-constant silica powder
CN106315591A (en) * 2016-08-25 2017-01-11 仇颖超 Method for preparing high-purity fused silica micropowder by composite plant acid
CN113798037A (en) * 2021-09-13 2021-12-17 苏州锐朗新材料有限公司 Raw material pretreatment process suitable for chip packaging materials with different attributes

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Application publication date: 20130515