CN105330177B - The method that laser selective sintering prepares seal glass prefabricated component - Google Patents
The method that laser selective sintering prepares seal glass prefabricated component Download PDFInfo
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- CN105330177B CN105330177B CN201510849674.3A CN201510849674A CN105330177B CN 105330177 B CN105330177 B CN 105330177B CN 201510849674 A CN201510849674 A CN 201510849674A CN 105330177 B CN105330177 B CN 105330177B
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- prefabricated component
- seal glass
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- pelletizing
- selective sintering
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Abstract
The invention discloses a kind of method that laser selective sintering prepares seal glass prefabricated component, comprise the following steps：(1) parent glass material is prepared；Described parent glass material particle diameter≤40 μm；(2) it is 90 99 according to mass ratio by the parent glass material and organic binder bond：1 10 mixing granulations are prepared into pelletizing, described pelletizing particle diameter≤100 μm；(3) pelletizing is subjected to laser selective sintering, prepares seal glass prefabricated component：Described pelletizing is carried out continuously n tiling and sintered and produces described seal glass prefabricated component；The tiling thickness of the pelletizing is 50 500 μm, and the height of described n values prefabricated component needed for selects；Described laser sintered power is 10 100W, and laser beam focus size is 0.01 0.1mm.The inventive method improves the production efficiency and yield rate of seal glass prefabricated component without using mould.
Description
Technical field
The present invention relates to glass processing field, and in particular to a kind of laser selective sintering prepares seal glass prefabricated component
Method.
Background technology
Seal glass prefabricated component is that glass powder is pressed into required shape, and turning into after dumping, pre- porcelain has necessarily
The sintered body of intensity, it can simplify device process for sealing, improve sealing-in precision.Seal glass prefabricated component have bond strength it is high,
Good chemical stability, available for the insulation air-tight packaging of optical window, optical fiber, alloy in lightweight, electric connector etc., it is
One of supporting basic material in the fields such as photodetector, sensor, electric connector.
The method of generally use molding sintering prepares seal glass prefabricated component at present, and molding sintering can meet most of pre-
The production requirement of product, but be difficult to produce miniature and complicated shape prefabricated component in batches：Miniature prefabricated component mould therefor size is small, pole
Fragile, processing, maintenance cost are high, and the quality stability of unmanageable base substrate；For complicated shape prefabricated component, there is also
Base substrate easy buckling deformation when dumping, pre- porcelain, the problems such as accuracy to size is not high, yield rate is extremely low.These production problems, resistance
The research and development process of Related product is hindered.
The content of the invention
It is an object of the invention to provide a kind of method that laser selective sintering prepares seal glass prefabricated component, it is used
Pelletizing is prepared into seal glass prefabricated component by laser selective sintering, is solved existing for common mould pressing method production prefabricated component
The problems such as difficult forming, precision are low, mould loss is big.
The purpose of the present invention is achieved by the following technical solution：
The invention provides a kind of method that laser selective sintering prepares seal glass prefabricated component, comprise the following steps：
(1) parent glass material is prepared；Described parent glass material particle diameter≤40 μm；
(2) it is 90-99 according to mass ratio by the parent glass material and organic binder bond：1-10 mixing granulations, which are prepared into, to be made
Grain powder, described pelletizing particle diameter≤100 μm；
(3) pelletizing is subjected to laser selective sintering, prepares seal glass prefabricated component：Described pelletizing is connected
It is continuous to carry out n tiling and sinter to produce described seal glass prefabricated component；
The tiling thickness of the pelletizing is 50-500 μm, and the height of described n values prefabricated component needed for selects；Institute
The laser sintered power stated is 10-100W, and laser beam focus size is 0.01-0.1mm.
Further, described seal glass prefabricated component is subjected to heating dumping, to exclude organic binder bond therein.
Further, described parent glass material is mixed by parent glass powder and functional material powder；
Using described parent glass material quality as 100%, wherein, described functional material powder quality fraction≤60%；
The functional material powder includes negative expansion ceramic powders, low dielectric constant ceramic powder.
Further, described laser selective is sintered under condition of negative pressure and carried out, wherein air pressure≤0.05MPa.
Further, the laser power 20-50W, laser beam focus size 0.05-0.08mm.
Further, the laser selective sintering is carried out in a heated condition, heating-up temperature≤500 DEG C.
Further, described heating is using infrared heating, heat radiation heating or heating plate heat transfer.
Further, described parent glass material particle diameter is 5-20 μm.
Further, described pelletizing is made of mist projection granulating or by hand granulation.
Further, described organic binder bond is any one in polyvinyl alcohol, polyethylene glycol, paraffin and terpinol
Kind.
Compared with prior art, the preparation method of seal glass prefabricated component of the present invention at least possesses following advantage：
Laser selective sintering technology to the successively sintering of pelletizing by preparing seal glass prefabricated component, it is not necessary to any
Mould, can process simplification, shorten lead time of product, eliminate the cost of mould.
The near-net-shape mode of laser selective sintering still rapidly and efficiently, it is possible to reduce waste of material；Laser selective
Sintering technology solves the technical barrier that miniature, complicated shape prefabricated component is difficult to be molded, be difficult to sintering porcelain, lifts extraordinary sealing-in glass
The production technology level of glass prefabricated component, porous, ultra-thin, super large prefabricated component production efficiency and yield rate can be improved.
Brief description of the drawings
Fig. 1 is that laser selective sintering of the present invention prepares a kind of seal glass prefabricated component in the method for seal glass prefabricated component
Sinter pattern；
It is prefabricated that Fig. 2 is that laser selective sintering of the present invention prepares another seal glass in the method for seal glass prefabricated component
Part sinters pattern.
Embodiment
It is convenient to understand to make the goal of the invention of the present invention, technical scheme and technique effect clearer, with reference to this hair
Bright preferred embodiment is described in further detail, but not as limiting to the invention.
Embodiment 1
A kind of preparation method of seal glass prefabricated component, comprises the following steps：
(1) first by 700g PbO-ZnO-B2O3Low temperature sealing glass grinds to obtain below 20 μm of particle diameter through melting, quenching
Powder, with the Ca below 20 μm of 300g particle diametersxPb1-xTiO3Filler powder uniformly mixes, and composite foundation frit is made；
PbO-ZnO-B wherein used2O3Seal glass is made up of the component of following mass fraction：PbO：35%；ZnO：
26%；B2O3：37%；Dirt：2%；
Ca thereinxPb1-xTiO3Filler powder has excellent chemical stability and excellent negative thermal expansion, reduces sealing-in
The coefficient of expansion of glass simultaneously improves its mechanical property；
The particle diameter that the particle diameter of powder is excessive will to cause pelletizing is excessive, is beaten because the excessive pelletizing of particle diameter is unfavorable for 3D
The sintering of print, it is therefore desirable to sieved, particle diameter crosses the waste that conference causes raw material.
(2) 50g paraffin is added in composite foundation frit obtained in the previous step, heating stirring, granulation are simultaneously sieved, and are made
Obtain the pelletizing of 400 mesh (38 μm of particle diameter) below；
The excessive effect that will influence sintering of the particle diameter of pelletizing, high is required to the condition of printing, it is difficult to operate, and can make
It is difficult to be molded into prefabricated component.
(3) selective laser sintering is carried out using above-mentioned pelletizing, every layer graphic printing, dash area are as shown in Figure 1
Selective laser sintering region, pass through successively powdering, sintering, every layer of powdering thickness 0.1mm, continuous 30 layers of paving.
From CO2Laser, power 40W, focal beam spot 0.1mm, operating room vacuumize, vacuum 0.2MPa.
Herein it should be noted that：Power is too low or focused radius can reduce greatly the cost of sintering, but accordingly
Occur that the sinter molding of seal glass prefabricated component is difficult, only select suitable power and focal beam spot both to reach sintering
Effect saved cost again.
The focal beam spot of use is smaller, powdering thickness is thinner, pelletizing particle diameter is smaller, the seal glass prefabricated component of processing
Formed precision it is also higher, but focal beam spot be 0.01mm can meet high-precision seal glass prefabricated component will
Ask, continue reduce focal beam spot again can be to equipment requirement it is higher；Powdering thickness has been less than the raising of its sintering precision after 50 μm
Through unobvious, but the number of powdering can be caused to increase, and then extend sintering time.
Vacuum condition sinters the porosity that can reduce seal glass prefabricated component, improves sintering quality, but vacuum is too high again
The requirement to equipment can be caused higher, select suitable vacuum, on the premise of the porosity of requirement and sintering quality is reached
Printing cost is reduced as far as possible.
The preparation method of the seal glass prefabricated component of the present embodiment is without the use of mould, reduces complicated shape prefabricated component
It is molded difficulty；Improve porous, ultra-thin, super large prefabricated component production efficiency and yield rate.
Embodiment 2
A kind of preparation method of seal glass prefabricated component, comprises the following steps：
(1) first by 1kg Na2O-CaO-SiO2Glass melting is uniform based on the Canasite glass of-F systems obtains
To parent glass melt, by above-mentioned parent glass melt water quenching, screening obtains the granular parent glass that granularity is less than 40 μm
Material, above-mentioned granular parent glass material are in the majority with circular granular；
Its component is above-mentioned parent glass by mass percentage：SiO：65%；CaO：15%；K2O：12%；Al2O3：
3%；F：2%；Dirt：3%；
(2) 100g polyvinyl alcohol is added in parent glass material obtained in the previous step, then by the feed system of granulation tower
System is sent into granulation tower, carries out mist projection granulating, and sieves, and the pelletizing of 160 mesh (96 μm of particle diameter) below, the ball of mist projection granulating is made
Shape degree is high, good fluidity, is adapted to powdering；
Mist projection granulating arrange parameter is as follows：The production control parameter of wherein sponging granulator is as follows：Inlet temperature is 190
℃；Outlet temperature is 105 DEG C；Negative pressure is -5Pa in tower；Atomizer revolution is 7500rpm；Feed pump revolution is 21Hz.
The excessive effect that will influence sintering of the particle diameter of pelletizing, high is required to the condition of printing, it is difficult to operate, and can make
It is difficult to be molded into prefabricated component.
(3) selective laser sintering is carried out using above-mentioned pelletizing, every layer graphic printing, dash area are as shown in Figure 2
Selective laser sintering region, pass through successively powdering, sintering, every layer of powdering thickness 0.5mm, continuous 10 layers of paving.
From semiconductor laser, power 100W, focal beam spot 0.01mm, operating room is filled with argon gas.
The particle diameter of the pelletizing used due to the present embodiment is larger, if use power is small or focused radius big city
Cause sintering effect undesirable, under atmosphere of inert gases, the porosity of seal glass prefabricated component can be reduced, improve sealing-in glass
The quality of glass prefabricated component.
The seal glass prefabricated component that above-mentioned steps obtain is put into heating furnace and carries out heating dumping, increases seal glass
The intensity of prefabricated component.
The preparation method of the seal glass prefabricated component of the present embodiment is without the use of mould, reduces complicated shape prefabricated component
It is molded difficulty；Improve porous, ultra-thin, super large prefabricated component production efficiency and yield rate.
Embodiment 3
A kind of preparation method of seal glass prefabricated component, comprises the following steps：
(1) parent glass material is prepared：First by 400g PbO-ZnO-B2O3Low temperature sealing glass is ground through melting, quenching
The powder below 20 μm of particle diameter is obtained, is mixed with the low dielectric constant ceramic powder below 600g 20 μm of particle diameter and parent glass is made
Material；
PbO-ZnO-B wherein used2O3Seal glass is made up of the component of following mass fraction：PbO：20%；ZnO：
32%, B2O3：45%；Dirt：3%；
(2) 100g terpinols and above-mentioned parent glass material mixing granulation are prepared into pelletizing, described pelletizing particle diameter
≤100μm；It is granulated and is granulated using manual, it is low for equipment requirements, it is easy to operate, it is suitable for the research in laboratory；
(3) pelletizing is subjected to laser selective sintering, prepares seal glass prefabricated component：Described pelletizing is pressed
It is carried out continuously 18 tilings for 50 μm according to each tiling thickness and sinters and produces described seal glass prefabricated component；
The laser sintered power used is sintered as 10W, laser beam focus size is 0.1mm, air pressure 0.03MPa, is used
Infrared heating, 300 DEG C of heating-up temperature；The heating properties of infrared heating are stable.
Embodiment 4
A kind of preparation method of seal glass prefabricated component, comprises the following steps：
(1) parent glass material is prepared：First by 800g PbO-ZnO-B2O3Low temperature sealing glass is ground through melting, quenching
The powder below 40 μm of particle diameter is obtained, is mixed with the negative expansion ceramic powders below 200g 40 μm of particle diameter and parent glass is made
Material；
PbO-ZnO-B wherein used2O3Seal glass is made up of the component of following mass fraction：PbO：29%；ZnO：
25%；B2O3：42%；Dirt：4%；
(2) 100g terpinols and above-mentioned parent glass material mixing granulation are prepared into pelletizing, described pelletizing particle diameter
≤100μm；It is granulated and is granulated using manual, it is low for equipment requirements, it is easy to operate, it is suitable for the research in laboratory；
(3) pelletizing is subjected to laser selective sintering, prepares seal glass prefabricated component：Described pelletizing is pressed
It is carried out continuously 10 tilings for 200 μm according to each tiling thickness and sinters and produces described seal glass prefabricated component；
The laser sintered power used is sintered as 100W, laser beam focus size is 0.02mm, air pressure 0.03MPa, is adopted
With infrared heating, 500 DEG C of heating-up temperature；The heating properties of infrared heating are stable.
Because powdering particle diameter is larger, it is therefore desirable to use higher sintering power and less focal dimension, otherwise can make
Slower into sinter molding, molding effect is bad, contributes to the sinter molding of prefabricated component using infrared heating, can be with vacuum condition
The porosity of seal glass prefabricated component is reduced, improves sintering quality.
Not most part in the present patent application, is that those skilled in the art select conventional technique according to common sense in the field
It can complete, as that can select short-pulse laser heating, heat radiation heating and heating plate heat transfer etc. different as needed
Mode of heating；If less demanding, sintering can be carried out at ambient pressure etc..
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of method that laser selective sintering prepares seal glass prefabricated component, it is characterised in that comprise the following steps：
(1) parent glass material is prepared；Described parent glass material particle diameter≤40 μm；
Wherein, described parent glass material is mixed by parent glass powder and functional material powder；With described basic glass
Glass material quality is 100%, wherein, described functional material powder quality fraction≤60%；
(2) it is 90-99 according to mass ratio by the parent glass material and organic binder bond：1-10 mixing granulations are prepared into granulation
Powder, described pelletizing particle diameter≤100 μm；
(3) pelletizing is subjected to laser selective sintering, prepares seal glass prefabricated component：Described pelletizing is continuously entered
The tiling of row n times and sinter and produce described seal glass prefabricated component；
The tiling thickness of the pelletizing is 50-500 μm, and the height of described n values prefabricated component needed for selects；Described
Laser sintered power is 10-100W, and laser beam focus size is 0.01-0.1mm.
2. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that will
Described seal glass prefabricated component carries out heating dumping, to exclude organic binder bond therein.
3. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that institute
Stating functional material powder includes negative expansion ceramic powders, low dielectric constant ceramic powder.
4. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that institute
The laser selective stated is sintered under condition of negative pressure and carried out, wherein air pressure≤0.05MPa.
5. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that institute
State laser power 20-50W, laser beam focus size 0.05-0.08mm.
6. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that institute
State laser selective sintering to carry out in a heated condition, heating-up temperature≤500 DEG C.
7. the method that laser selective sintering according to claim 6 prepares seal glass prefabricated component, it is characterised in that institute
The heating stated is using infrared heating, heat radiation heating or heating plate heat transfer.
8. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that institute
The parent glass material particle diameter stated is 5-20 μm.
9. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that institute
The pelletizing stated is made of mist projection granulating or by hand granulation.
10. the method that laser selective sintering according to claim 1 prepares seal glass prefabricated component, it is characterised in that
Described organic binder bond is any one in polyvinyl alcohol, polyethylene glycol, paraffin and terpinol.
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| CN106277724B (en) * | 2016-08-23 | 2019-06-14 | 中国建筑材料科学研究总院 | The method that laser selective sintering prepares glassware |
| CN114656167A (en) * | 2022-03-21 | 2022-06-24 | 湖南大学 | Glass connecting method and device based on glass frit |
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| CN102093646B (en) * | 2010-10-29 | 2012-07-18 | 华南理工大学 | Material for rapid three dimensional printing forming and preparation method thereof |
| CN103073174A (en) * | 2013-02-19 | 2013-05-01 | 苏州百纳思光学科技有限公司 | 3D laser printing device taking low-melting-point glass powder as raw material |
| CN103936392B (en) * | 2014-03-13 | 2015-07-08 | 济南大学 | Preparation method of 3D printing inorganic powder molding material |
| CN104944750A (en) * | 2014-03-25 | 2015-09-30 | 郭作超 | Glass 3D printing device |
| CN104647760B (en) * | 2015-02-12 | 2017-03-08 | 华中科技大学 | A kind of 3D printing manufacture method of short fiber reinforced thermosetting resin joint product |
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