CN103194632B - Preparation method of high-volume fraction micrometer alumina ceramic enhanced composite material - Google Patents
Preparation method of high-volume fraction micrometer alumina ceramic enhanced composite material Download PDFInfo
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- CN103194632B CN103194632B CN201310158233.XA CN201310158233A CN103194632B CN 103194632 B CN103194632 B CN 103194632B CN 201310158233 A CN201310158233 A CN 201310158233A CN 103194632 B CN103194632 B CN 103194632B
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- stove
- thermal compression
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Abstract
The invention provides a preparation method of a high-volume fraction micrometer alumina ceramic enhanced composite material. The preparation method is characterized by sequentially comprising the steps of material mixing, cold pressing and densification sintering and avoiding the shortcomings of equipment complexity, high construction cost, long production period and high energy consumption.
Description
Technical field
The present invention relates to the preparing technical field that a kind of high-volume fractional micrometer alumina pottery strengthens aluminum composite, particularly relates to a kind of discharge plasma sintering legal system that utilizes and strengthens the method for aluminum composite for high-volume fractional micrometer alumina pottery.
Background technology
Ceramic particle reinforced aluminium base composite material has the high physicals more excellent than strong, Gao Bimo, wear resistance and low thermal expansivity etc., be widely used in aerospace, military field and the industry such as automobile, electronic instrument, as aluminum matrix composite has successfully been used in power device base or heat sink, printed circuit board (PCB) core and the encapsulation of microprocessor end cap by U.S. Lanxide and Japanese Sumitomo electronics corporation.Present stage, the general ceramic performs infiltration process that adopts can prepare the particle enhanced aluminum-based composite material that volume fraction is 55% ~ 70%, has described the operation steps of these class methods in patent CN 102191398 A in detail.But the shortcomings such as the method exists equipment complexity, involve great expense or the production cycle is long.
Adopt powder metallurgy also can prepare the aluminum matrix composite of high-volume fractional ceramic particle content.If directly the ceramic particle of high-volume fractional is mixed with aluminum-based powder, usually need ceramic particle and the long-time high-energy ball milling of aluminum-based powder, to improve both mixing uniformity, and then improve and sinter power, the density of sintered article and homogeneity of structure into.This adds preparation cycle and power consumption to a certain extent.
Summary of the invention
The invention provides the preparation method that a kind of high-volume fractional micrometer alumina pottery strengthens aluminum composite, the feature of the method be successively through batch mixing, cold pressing and densification sintering process, avoid equipment complexity, involve great expense, the production cycle long and high shortcoming that consumes energy.
For achieving the above object, technical scheme of the present invention is:
High-volume fractional micrometer alumina pottery strengthens a preparation method for aluminum composite, and step is as follows:
Step 1: first by the volume fraction range preset, configure the mixed powder be made up of micron pure aluminium powder and micrometer alumina ceramics powder, mixed powder is inserted in mechanical mixer and carry out batch mixing operation to reach the object mixed, mixing time scope is 5 hours-10 hours, and the volume fraction of alumina-ceramic powder is v
0%, v
0span be 20 ~ 30;
Step 2: the part in the mixed powder after extracting batch mixing operation according to predetermined amount is also inserted in the hot pressing graphite jig of pre-set dimension size, first with hand, in advance block is pressed into the mixed powder after the batch mixing operation of inserting in the hot pressing graphite jig of pre-set dimension size, after being pressed into block in advance, mixed powder after compacting of carrying out colding pressing under 20 ~ 30MPa pressure range is pressed into block in advance, the time of colding pressing is 30 seconds ~ 90 seconds, measure the powder face height of the mixed powder after the compacting in hot pressing graphite jig after colding pressing, the value of this powder face height is h
0;
Step 3: according to the density value 3.9g/cm of ceramic particle
3, aluminium density value 2.7g/cm
3, mixed powder after compacting in graphite jig mass value m
0with hot pressing die inner diameter values d, be the sample rate under 0% condition after deriving 100% densification sintering of the mixed powder after this compacting and in the porosity of sintered specimen, and sample rate derive sintered sample thickness thus, sintered sample one-tenth-value thickness 1/10 h
1=[m
0/ (3.9 × v
0%+2.7 × (100-v
0) %)]/[3.14 × (d/2)
2], the massfraction obtaining aluminum oxide is like this w
0%=3.9 × v
0%/(3.9 × v
0%+2.7 × (100-v
0) %);
Step 4: the stove that the graphite thermal compression mould after colding pressing puts into discharge plasma sintering stove is carried out 100% densification sintering, this 100% densification sintering detailed process is the pressure graphite thermal compression mould after colding pressing being applied to 0.1MPa, after graphite thermal compression mould after colding pressing in the stove of discharge plasma sintering stove is warming up to 600 DEG C under vacuum conditions, heating power is regulated to make temperature rise to 660-730 DEG C by pre-set velocity again, after thermometer registration is steady, continue to make pressure head continue to be pressed in the graphite thermal compression mould after colding pressing according to pre-set velocity pressurization;
Step 5: continue to be pressed into the graphite thermal compression mould after colding pressing until press-in displacement is h at pressure head
0-h
1time, regulate pressure size to remain unchanged to make this press-in displacement, the time range keeping this press-in displacement state is 5-10 minute, and obtaining quality of alumina mark is w
0aluminum oxide/aluminum composite the c of %
0;
Step 6: calculating micrometer alumina grain volume fraction is v
1aluminum oxide/aluminum composite (the c of %
1) density be ρ
1=3.9 g/cm
3× v
1%+2.7 g/cm
3× (1-v
1%), v
1scope be 50 ~ 80, now matrix material c
1the massfraction of middle alumina ceramic grain is w
1%=3.9 g/cm
3× v
1%/ρ
1.Calculating utilizes matrix material c
0for parent material prepares matrix material c
1, needing to remove quality is Δ m=(m
0× w
1%-m
0× w
0%)/w
1the aluminium of %, derives the press-in shift value h that pressure head continues to press down
2for Δ m/ (2.7g/cm
3× 3.14 × 3.1cm × 3.1cm) cm;
Step 7: continue graphite thermal compression mould raised temperature to 740 ~ 790 DEG C after colding pressing in the stove of discharge plasma sintering stove, until after thermometer registration is steady, then pressurization makes pressure head continue to go deep in graphite thermal compression mould according to the speed preset, so just make aluminium liquid be extruded from the gap of graphite thermal compression mould, the press-in shift value continuing to press down when pressure head is h
2time, also namely total press-in shift value is h
0-h
1+ h
2, the press-in shift value regulating pressure size to make described pressure head continue to press down remains unchanged, and the duration ranges remained unchanged is 5 ~ 10 minutes;
Step 8: stop subsequently heating in the stove of discharge plasma sintering stove, makes the furnace temperature in the stove of discharge plasma sintering stove carry out Temperature fall, and regulates pressure size to keep total press-in shift value constant in h
0-h
1+ h
2, until when temperature is down to below 100 DEG C, lay down the furnace pressure of discharge plasma sintering stove, the sample obtained after blow-on sampling is the aluminum matrix composite that ceramic particle volume fraction range is 50-80%.
The feature that the feature of the inventive method is be successively through batch mixing, cold pressing and densification sintering process, avoid equipment complexity, involve great expense, the production cycle long and high shortcoming that consumes energy.And there is simple to operate and that cost is low advantage.
Embodiment
Below by specific embodiment, the present invention will be further described:
High-volume fractional micrometer alumina pottery strengthens the preparation method of aluminum composite, and step is as follows:
Step 1: first by the volume fraction range preset, configure by median size to be the pure aluminium powder of 60 microns and median size be mixed powder that the alumina-ceramic powder of 60 microns forms, mixed powder is inserted in mechanical mixer and carry out batch mixing operation to reach the object mixed, mixing time scope is 5 hours, in order to make powder mix, the volume fraction of alumina-ceramic powder is v
0%, v
0value be 30;
Step 2: extract the mixed powder after the operation of 92.4g batch mixing, and inserted in the hot pressing graphite jig of pre-set dimension size, the inner cavity size of hot pressing graphite jig is Ф 62mm × 60mm and graphite seaming chuck height is 65mm, first with hand, in advance block is pressed into the mixed powder after the batch mixing operation of inserting in the hot pressing graphite jig of pre-set dimension size, after being pressed into block in advance, mixed powder after compacting of carrying out colding pressing under 30MPa pressure range is pressed into block in advance, the time of colding pressing is 60 seconds, the powder face height of the mixed powder after the compacting in hot pressing graphite jig is measured after colding pressing, the value of this powder face height is h
0=20mm,
Step 3: according to the density value 3.9g/cm of ceramic particle
3, aluminium density value 2.7g/cm
3, mixed powder after compacting in graphite jig mass value m
0with hot pressing die inner diameter values d, be the sample rate under 0% condition after deriving 100% densification sintering of the mixed powder after this compacting and in the porosity of sintered specimen, and sample rate derive sintered sample thickness thus, sintered sample one-tenth-value thickness 1/10 h
1=10mm, the massfraction obtaining aluminum oxide is like this w
0%=38.24%;
Step 4: the stove that the graphite thermal compression mould after colding pressing puts into discharge plasma sintering stove is carried out 100% densification sintering, this 100% densification sintering detailed process is the pressure graphite thermal compression mould after colding pressing being applied to 0.1MPa, after graphite thermal compression mould after colding pressing in the stove of discharge plasma sintering stove is warming up to 600 DEG C under vacuum conditions, heating power is regulated to make temperature rise to 660-730 DEG C by pre-set velocity again, after thermometer registration is steady, continue to make pressure head continue to be pressed in the graphite thermal compression mould after colding pressing according to pre-set velocity pressurization;
Step 5: continue to be pressed into the graphite thermal compression mould after colding pressing until press-in displacement is h at pressure head
0-h
1during=10cm, regulate pressure size to remain unchanged to make this press-in displacement, the time range keeping this press-in displacement state is 5-10 minute, and obtaining quality of alumina mark is w
0aluminum oxide/aluminum composite the c of %
0;
Calculating micrometer alumina grain volume fraction is v
1aluminum oxide/aluminum composite (the c of %
1) density be ρ
1=3.9 g/cm
3× v
1%+2.7 g/cm
3× (1-v
1%), v
1scope be 50 ~ 80, now matrix material c
1the massfraction of middle alumina ceramic grain is w
1%=3.9 g/cm
3× v
1%/ρ
1.Calculating utilizes matrix material c
0for parent material prepares matrix material c
1, needing to remove quality is Δ m=(m
0× w
1%-m
0× w
0%)/w
1the aluminium of %, derives the press-in shift value h that pressure head continues to press down
2for Δ m/ (2.7g/cm
3× 3.14 × 3.1cm × 3.1cm) cm;
Step 6: calculating micrometer alumina grain volume fraction is v
1aluminum oxide/aluminum composite (the c of %
1) density be ρ
1=3.15g/cm
3, v
1value be 60, now matrix material c
1the massfraction of middle alumina ceramic grain is w
1%=74.3%.Calculating utilizes matrix material c
0for parent material prepares matrix material c
1, need to remove the aluminium that quality is Δ m=44.85g, derive the press-in shift value h that pressure head continues to press down
2for 5.5cm;
Step 7: continue graphite thermal compression mould raised temperature to 740 ~ 790 DEG C after colding pressing in the stove of discharge plasma sintering stove, until after thermometer registration is steady, then pressurization makes pressure head continue to go deep in graphite thermal compression mould according to the speed preset, aluminium liquid is so just made to be extruded from the gap of graphite thermal compression mould, when the press-in shift value that pressure head continues to press down is 5.5mm, also namely total press-in shift value is 15.5mm, the press-in shift value regulating pressure size to make described pressure head continue to press down remains unchanged, the duration ranges remained unchanged is 5 ~ 10 minutes,
Step 8: stop subsequently heating in the stove of discharge plasma sintering stove, the furnace temperature in the stove of discharge plasma sintering stove is made to carry out Temperature fall, and regulate pressure size to keep total press-in shift value constant in 15.5mm, until when temperature is down to below 100 DEG C, lay down the furnace pressure of discharge plasma sintering stove, the sample obtained after blow-on sampling is the aluminum matrix composite that ceramic particle volume fraction range is 60%, and its density is 3.15g/cm
3, error is less than 5%.
The above; it is only the embodiment that the present invention is directed to the inventive method; above-described embodiment not does any restriction to the present invention; every scope given by technical solution of the present invention and to any simple modification made for any of the above embodiments, change and equivalent structure change, all still belongs to the protection domain of technical solution of the present invention.
Claims (1)
1. high-volume fractional micrometer alumina pottery strengthens a preparation method for aluminum composite, and it is characterized in that, step is as follows:
Step 1: first by the volume fraction range preset, configure the mixed powder be made up of micron pure aluminium powder and micrometer alumina ceramics powder, mixed powder is inserted in mechanical mixer and carry out batch mixing operation to reach the object mixed, mixing time scope is 5 hours-10 hours, and the volume fraction of alumina-ceramic powder is v
0%, v
0span be 20 ~ 30;
Step 2: the part in the mixed powder after extracting batch mixing operation according to predetermined amount is also inserted in the hot pressing graphite jig of pre-set dimension size, first with hand, in advance block is pressed into the mixed powder after the batch mixing operation of inserting in the hot pressing graphite jig of pre-set dimension size, after being pressed into block in advance, mixed powder after compacting of carrying out colding pressing under 20 ~ 30MPa pressure range is pressed into block in advance, the time of colding pressing is 30 seconds ~ 90 seconds, measure the powder face height of the mixed powder after the compacting in hot pressing graphite jig after colding pressing, the value of this powder face height is h
0;
Step 3: according to the density value 3.9g/cm of ceramic particle
3, aluminium density value 2.7g/cm
3, mixed powder after compacting in graphite jig mass value m
0with hot pressing die inner diameter values d, be the sample rate under 0% condition after deriving 100% densification sintering of the mixed powder after this compacting and in the porosity of sintered specimen, and sample rate derive sintered sample thickness thus, sintered sample one-tenth-value thickness 1/10
, the massfraction obtaining aluminum oxide is like this
;
Step 4: the stove that the graphite thermal compression mould after colding pressing puts into discharge plasma sintering stove is carried out 100% densification sintering, this 100% densification sintering detailed process is the pressure graphite thermal compression mould after colding pressing being applied to 0.1MPa, after graphite thermal compression mould after colding pressing in the stove of discharge plasma sintering stove is warming up to 600 DEG C under vacuum conditions, heating power is regulated to make temperature rise to 660-730 DEG C by pre-set velocity again, after thermometer registration is steady, continue to make pressure head continue to be pressed in the graphite thermal compression mould after colding pressing according to pre-set velocity pressurization;
Step 5: continue to be pressed into the graphite thermal compression mould after colding pressing until press-in displacement is h at pressure head
0-h
1time, regulate pressure size to remain unchanged to make this press-in displacement, the time range keeping this press-in displacement state is 5-10 minute, and obtaining quality of alumina mark is w
0aluminum oxide/aluminum composite the c of %
0;
Step 6: calculating micrometer alumina grain volume fraction is v
1aluminum oxide/aluminum composite (the c of %
1) density be
, v
1scope be 50 ~ 80, now matrix material c
1the massfraction of middle alumina ceramic grain is
, calculate and utilize matrix material c
0for parent material prepares matrix material c
1, need remove quality be
aluminium, derive pressure head and continue the press-in shift value h that presses down
2for
;
Step 7: continue graphite thermal compression mould raised temperature to 740 ~ 790 DEG C after colding pressing in the stove of discharge plasma sintering stove, after thermometer registration is steady, then pressurization makes pressure head continue to go deep in graphite thermal compression mould according to the speed preset, so just make aluminium liquid be extruded from the gap of graphite thermal compression mould, the press-in shift value continuing to press down when pressure head is h
2time, also namely total press-in shift value is h
0-h
1+ h
2, the press-in shift value regulating pressure size to make described pressure head continue to press down remains unchanged, and the duration ranges remained unchanged is 5 ~ 10 minutes;
Step 8: stop subsequently heating in the stove of discharge plasma sintering stove, makes the furnace temperature in the stove of discharge plasma sintering stove carry out Temperature fall, and regulates pressure size to keep total press-in shift value constant in h
0-h
1+ h
2, until when temperature is down to below 100 DEG C, lay down the furnace pressure of discharge plasma sintering stove, the sample obtained after blow-on sampling is the aluminum matrix composite that ceramic particle volume fraction range is 50-80%.
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|---|---|---|---|
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|---|---|---|---|
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| CN103194632B true CN103194632B (en) | 2015-04-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106392099B (en) * | 2016-06-08 | 2018-08-31 | 昆明理工大学 | A kind of preparation method of aluminium oxide/aluminium composite superfine powder |
| CN106077689B (en) * | 2016-06-08 | 2018-05-25 | 昆明理工大学 | A kind of preparation method of sheet cross-linked structure aluminium oxide/aluminium composite granule |
| CN109304558B (en) * | 2018-11-08 | 2021-01-05 | 桂林航天工业学院 | Based on micron Al2O3Composite aluminum-based brazing wire and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472354A (en) * | 2002-07-31 | 2004-02-04 | ������ɫ�����о���Ժ | Particle reinforced aluminium-based composite material and workpiece therefrom and its forming process |
| CN1810419A (en) * | 2006-03-01 | 2006-08-02 | 中国科学院上海硅酸盐研究所 | Prepn process of composite aluminium/alumina material with alumina coated metal aluminium |
| CN102212722A (en) * | 2011-05-09 | 2011-10-12 | 河南理工大学 | Preparation method of particle-reinforced aluminum-base composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH042703A (en) * | 1990-04-18 | 1992-01-07 | Kobe Steel Ltd | Manufacture of al-base composite material |
| DE10203283C5 (en) * | 2002-01-29 | 2009-07-16 | Gkn Sinter Metals Gmbh | Method for producing sintered components from a sinterable material and sintered component |
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2013
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472354A (en) * | 2002-07-31 | 2004-02-04 | ������ɫ�����о���Ժ | Particle reinforced aluminium-based composite material and workpiece therefrom and its forming process |
| CN1810419A (en) * | 2006-03-01 | 2006-08-02 | 中国科学院上海硅酸盐研究所 | Prepn process of composite aluminium/alumina material with alumina coated metal aluminium |
| CN102212722A (en) * | 2011-05-09 | 2011-10-12 | 河南理工大学 | Preparation method of particle-reinforced aluminum-base composite material |
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Effective date of registration: 20180328 Address after: 710075 Shaanxi province Xi'an city road high tech Zone Tang Tang Xing digital room 433 No. 6 Patentee after: Xi'an Zhuxi Technical Manager Technology Co., Ltd. Address before: Howking Weiyang Road No. 136 building, 710016 Shaanxi city of Xi'an province 10 Patentee before: Xi'an Zhuoxi New Material Technology Co., Ltd. |
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