CN107417127A - A kind of 3D printing glass powder, preparation method thereof - Google Patents

A kind of 3D printing glass powder, preparation method thereof Download PDF

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Publication number
CN107417127A
CN107417127A CN201710646902.6A CN201710646902A CN107417127A CN 107417127 A CN107417127 A CN 107417127A CN 201710646902 A CN201710646902 A CN 201710646902A CN 107417127 A CN107417127 A CN 107417127A
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China
Prior art keywords
glass
powder
printing
preparation
mixed
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CN201710646902.6A
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Chinese (zh)
Inventor
徐忠
张学兵
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Anhui Motivity Productivity Promotion Center Co Ltd
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Anhui Motivity Productivity Promotion Center Co Ltd
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Priority to CN201710646902.6A priority Critical patent/CN107417127A/en
Publication of CN107417127A publication Critical patent/CN107417127A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/02—Pretreated ingredients

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of 3D printing glass powder, preparation method thereof, the calcining heat is 495 DEG C, calcination time 8.5h, described PbO, NH4VO3、H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10:30, the clear glass of the shaping is to be shaped as square, circular or polygon, sieved to obtain safety glass powder with 400 mesh sieve after the glass breaking, grinding, it is easy to the later stage to print, described that mixed powder is ground, the grinding is carried out by the way of ball milling, is sufficiently mixed epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder, the present invention adds a kind of new glass printed material for 3D printing industry, promotes the development of 3D printing technique.

Description

A kind of 3D printing glass powder, preparation method thereof
Technical field
The invention belongs to 3D printing field, it is more particularly related to a kind of 3D printing glass powder, preparation method thereof.
Background technology
3D printing, it is according to designed 3D models, material is successively increased by 3D printing equipment to manufacture three-dimensional objects Technology.3D printing combines many necks such as digital modeling techniques, Electromechanical Control technology, information technology, material science and chemistry The cutting edge technology in domain, it is one kind of rapid shaping technique, is described as the core technology of " the third time industrial revolution ".With it is conventionally manufactured Technology is compared, and 3D printing need not manufacture mould in advance, it is not necessary to substantial amounts of material is removed in the fabrication process, also without going through complexity Forging technology can be obtained by final products, therefore, can be realized in production structure optimization, save material and save energy Source.3D printing technique is suitable for new product development, quick-acting single and parts in small batch manufacture, the manufacture of complicated shape part, mould Design and manufacture of tool etc., are also suitable for manufacture, configuration design inspection, assembly test of difficult-to-machine material etc..Therefore, 3D printing Industry receives concern more and more extensive both at home and abroad, will turn into next tool rising industry with broad prospects for development.
At present, 3D printing is applied to the fields such as product prototype, Making mold, art creation product, jewelry-making, can replace The conventional fine processing technology relied on for these fields.3D printing can largely lift the efficiency and precision of making Degree.In addition, also opened up more for it in the field such as bioengineering and medical science, building, clothes, the introducing of 3D printing technique Wide development space.Based on the strategic height of 21 century manufacturing industry competition, the U.S., Europe and Japan are all to RP technique Substantial amounts of research has been put into, has been developed rapidly 3D printing technique.In national defence, European and American developed countries pay much attention to 3D The application of printing technique, and put into huge fund and develop increasing material manufacturing metallic element, particularly promote increases material manufacturing technology to exist energetically Application in the manufacture of the high value material such as titanium alloy parts.
3D printing material is the important substance basis of 3D printing technique development, and to a certain extent, the development of material determines Can 3D printing the problem of broader applications.At present, 3D printing material mainly includes engineering plastics, photosensitive resin, rubber Class material, metal material and ceramic material etc., in addition, coloured plaster material, artificial bone meal, cell biological raw material and sand The food materials such as sugar are also applied in 3D printing field.These raw material used in 3D printing are all specific to 3D printing Equipment and technique and research and develop, it is otherwise varied with common plastics, gypsum, resin etc., its form typically have it is powdered, thread, The mouth such as lamellar, liquid.Generally, beaten according to the type of printing device and the difference of operating condition, used powdered 3D The particle diameter for printing material is 1~100 μm, and in order that powder keeps good mobility, typically require that powder there will be height Sphericity.This greatly restricts the development of 3D printing technique.
The content of the invention
Problem to be solved by this invention is to provide a kind of 3D printing glass powder, preparation method thereof.
To achieve these goals, the technical scheme taken of the present invention is：
A kind of 3D printing glass powder, preparation method thereof, comprises the following steps：
(1) prepared by glass fibre
Glass fibre is infiltrated using coupling agent 560, just level fiberglass is made；
(2) calcine
By kaolin, mountain tallow powder, magnesium hydroxide, silica, chromium oxide, rare earth oxide, nano aluminum, first level fiberglass Mixed with water, mixing temperature is 15-35 DEG C, incorporation time 40-60min, is then calcined so that calcined product is made；
(3) melt
By calcined product with by PbO, NH4VO3、H3BO3、Al2O3、SiO2、R2CO3Fully ground in mortar with calcined product Mill, melted after well mixed, 1100 DEG C -1200 DEG C of fusion temperature, be incubated 1-2 hours, obtain glass metal；
(4) it is molded
Glass metal is poured into graphite jig and is molded, the glass that cast obtains is placed in annealing furnace, at 300 DEG C -500 DEG C Lower annealing 1-2 hours, clear glass is obtained after cooling to room temperature with the furnace；
(5) tempering
Clear glass is put into tempering in annealing furnace or is put into bending tempering in bending annealing furnace, obtains plane or curve tempering Glass material, and crush, grind；
(6) mix
By resulting glass dust, epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder are mixed outside, it is fully mixed Close, obtain the glass dust for 3D printing；
Preferably, step (2) calcining heat is 470-520 DEG C, calcination time 7-10h.
Preferably, described step (3) PbO, NH4VO3、H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10: 4:14:10:30。
Preferably, the clear glass of step (4) shaping is to be shaped as square, circular or polygon.
Preferably, the step (5) will be sieved to obtain safety glass powder after glass breaking, grinding with 400 mesh sieve.
Preferably, it is preferred that the step (6) is ground to mixed powder, and the grinding uses ball milling method Carry out.
Preferably, the condition of step (6) ball milling is：The mass ratio of big ball and bead is 2：1.3-1.5, abrading-ball and thing The mass ratio of material is 10：0.8-1.2, rotating speed 600-1200rpm, Ball-milling Time 25-35min.
Beneficial effect：The invention provides a kind of 3D printing glass powder, preparation method thereof, the calcining heat is 495 DEG C, Calcination time is 8.5h, described PbO, NH4VO3、H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10: 30, the clear glass of the shaping is is shaped as square, circular or polygon, with 400 mesh after the glass breaking, grinding Sieve is sieved to obtain safety glass powder, is easy to the later stage to print, described that mixed powder is ground, and the grinding is adopted Carried out with the mode of ball milling, be sufficiently mixed epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder, the present invention is 3D Printing industry adds a kind of new glass printed material, promotes the development of 3D printing technique.
Embodiment
Embodiment 1：
A kind of 3D printing glass powder, preparation method thereof, comprises the following steps：
(1) prepared by glass fibre
Glass fibre is infiltrated using coupling agent 560, just level fiberglass is made；
(2) calcine
By kaolin, mountain tallow powder, magnesium hydroxide, silica, chromium oxide, rare earth oxide, nano aluminum, first level fiberglass Mixed with water, mixing temperature is 15 DEG C, incorporation time 40min, is then calcined so that calcined product is made, described to forge It is 470 DEG C to burn temperature, calcination time 7h；
(3) melt
By calcined product with by PbO, NH4VO3、H3BO3、Al2O3、SiO2、R2CO3Fully ground in mortar with calcined product Mill, melted after well mixed, 1100 DEG C of fusion temperature, be incubated 1 hour, obtain glass metal, described PbO, NH4VO3、 H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10:30；
(4) it is molded
Glass metal is poured into graphite jig and is molded, the glass that cast obtains is placed in annealing furnace, annealed at 300 DEG C 1 hour, cool to the furnace after room temperature and obtain clear glass, the clear glass of the shaping for be shaped as square, it is circular or Polygon；
(5) tempering
Clear glass is put into tempering in annealing furnace or is put into bending tempering in bending annealing furnace, obtains plane or curve tempering Glass material, and crush, grind, sieved to obtain safety glass powder with 400 mesh sieve afterwards；
(6) mix
By resulting glass dust, epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder are mixed outside, it is fully mixed Close, obtain the glass dust for 3D printing, mixed powder is ground, the grinding is carried out using ball milling method, institute The condition for stating ball milling is：The mass ratio of big ball and bead is 2：1.3, the mass ratio of abrading-ball and material is 10：0.8, rotating speed is 600rpm, Ball-milling Time 25min；
Embodiment 2：
A kind of 3D printing glass powder, preparation method thereof, comprises the following steps：
(1) prepared by glass fibre
Glass fibre is infiltrated using coupling agent 560, just level fiberglass is made；
(2) calcine
By kaolin, mountain tallow powder, magnesium hydroxide, silica, chromium oxide, rare earth oxide, nano aluminum, first level fiberglass Mixed with water, mixing temperature is 25 DEG C, incorporation time 60min, is then calcined so that calcined product is made, described to forge It is 495 DEG C to burn temperature, calcination time 8.5h；
(3) melt
By calcined product with by PbO, NH4VO3、H3BO3、Al2O3、SiO2、R2CO3Fully ground in mortar with calcined product Mill, melted after well mixed, 1150 DEG C of fusion temperature, be incubated 1.5 hours, obtain glass metal, described PbO, NH4VO3、 H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10:30；
(4) it is molded
Glass metal is poured into graphite jig and is molded, the glass that cast obtains is placed in annealing furnace, annealed at 400 DEG C 1.5 hours, cool to the furnace after room temperature and obtain clear glass, the clear glass of the shaping for be shaped as square, it is circular or Person's polygon；
(5) tempering
Clear glass is put into tempering in annealing furnace or is put into bending tempering in bending annealing furnace, obtains plane or curve tempering Glass material, and crush, grind, sieved to obtain safety glass powder with 400 mesh sieve afterwards；
(6) mix
By resulting glass dust, epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder are mixed outside, it is fully mixed Close, obtain the glass dust for 3D printing, mixed powder is ground, the grinding is carried out using ball milling method, institute The condition for stating ball milling is：The mass ratio of big ball and bead is 2：1.4, the mass ratio of abrading-ball and material is 10：1.0, rotating speed is 900rpm, Ball-milling Time 30min；
Embodiment 3：
A kind of 3D printing glass powder, preparation method thereof, comprises the following steps：
(1) prepared by glass fibre
Glass fibre is infiltrated using coupling agent 560, just level fiberglass is made；
(2) calcine
By kaolin, mountain tallow powder, magnesium hydroxide, silica, chromium oxide, rare earth oxide, nano aluminum, first level fiberglass Mixed with water, mixing temperature is 35 DEG C, incorporation time 60min, is then calcined so that calcined product is made, described to forge It is 520 DEG C to burn temperature, calcination time 10h；
(3) melt
By calcined product with by PbO, NH4VO3、H3BO3、Al2O3、SiO2、R2CO3Fully ground in mortar with calcined product Mill, melted after well mixed, 1200 DEG C of fusion temperature, be incubated 2 hours, obtain glass metal, described PbO, NH4VO3、 H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10:30；
(4) it is molded
Glass metal is poured into graphite jig and is molded, the glass that cast obtains is placed in annealing furnace, annealed at 500 DEG C 2 hours, cool to the furnace after room temperature and obtain clear glass, the clear glass of the shaping for be shaped as square, it is circular or Polygon；
(5) tempering
Clear glass is put into tempering in annealing furnace or is put into bending tempering in bending annealing furnace, obtains plane or curve tempering Glass material, and crush, grind, sieved to obtain safety glass powder with 400 mesh sieve afterwards；
(6) mix
By resulting glass dust, epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder are mixed outside, it is fully mixed Close, obtain the glass dust for 3D printing, mixed powder is ground, the grinding is carried out using ball milling method, institute The condition for stating ball milling is：The mass ratio of big ball and bead is 2：1.5, the mass ratio of abrading-ball and material is 10：1.2, rotating speed is 1200rpm, Ball-milling Time 35min；
After process above, sample is taken out respectively, and measurement result is as follows：
Detection project Embodiment 1 Embodiment 2 Embodiment 3 Prior art index
Quality It is high It is high It is low Typically
Intensity It is low It is high It is high It is low
Impact resistance Typically It is good It is good Typically
It can be drawn according to above table data, when 2 parameter of embodiment, the quality of 3D printing glass dust and intensity is all It is better than prior art index, and impact resistance is more preferable, i.e., this condition is more beneficial for the preparation of 3D printing glass dust.
The invention provides a kind of 3D printing glass powder, preparation method thereof, the calcining heat is 495 DEG C, and calcination time is 8.5h, described PbO, NH4VO3、H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10:30, it is described into The clear glass of type is carried out to be shaped as square, circular or polygon after the glass breaking, grinding with 400 mesh sieve Screening obtains safety glass powder, is easy to the later stage to print, described that mixed powder is ground, and the grinding is using ball milling Mode is carried out, and is sufficiently mixed epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder, and the present invention is 3D printing industry A kind of new glass printed material is added, promotes the development of 3D printing technique.
Above-described is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention Protection domain.

Claims (7)

  1. A kind of 1. 3D printing glass powder, preparation method thereof, it is characterised in that：Comprise the following steps：
    (1) prepared by glass fibre
    Glass fibre is infiltrated using coupling agent 560, just level fiberglass is made；
    (2) calcine
    By kaolin, mountain tallow powder, magnesium hydroxide, silica, chromium oxide, rare earth oxide, nano aluminum, first level fiberglass and water Mixed, mixing temperature is 15-35 DEG C, incorporation time 40-60min, is then calcined so that calcined product is made；
    (3) melt
    By calcined product with by PbO, NH4VO3、H3BO3、Al2O3、SiO2、R2CO3It is fully ground, mixes in mortar with calcined product Melted after closing uniformly, 1100 DEG C -1200 DEG C of fusion temperature, be incubated 1-2 hours, obtain glass metal；
    (4) it is molded
    Glass metal is poured into graphite jig and is molded, the glass that cast obtains is placed in annealing furnace, moved back at 300 DEG C -500 DEG C Fiery 1-2 hours, clear glass is obtained after cooling to room temperature with the furnace；
    (5) tempering
    Clear glass is put into tempering in annealing furnace or is put into bending tempering in bending annealing furnace, obtains plane or curved strengthened glass Material, and crush, grind；
    (6) mix
    By resulting glass dust, epoxy resin, nano-zinc oxide powder and nano oxidized titanium powder are mixed outside, is sufficiently mixed, obtains To the glass dust for 3D printing；
    (7) print
    Forming temperature is room temperature, and sweep speed 800-1400m/s, laser power is under 8-14W, is beaten mixed for 3D The mode of the glass dust selective laser sintering of print, is successively printed, and can obtain glassware；
  2. 2. according to a kind of 3D printing glass powder, preparation method thereof described in claim 1, it is characterised in that：The step (2) is forged It is 470-520 DEG C to burn temperature, calcination time 7-10h.
  3. 3. according to a kind of 3D printing glass powder, preparation method thereof described in claim 1, it is characterised in that：The step (3) PbO、NH4VO3、H3BO3、Al2O3、SiO2Weight ratio with calcined product is 5:10:4:14:10:30.
  4. 4. according to a kind of 3D printing glass powder, preparation method thereof described in claim 3, it is characterised in that：The step (4) into The clear glass of type is to be shaped as square, circular or polygon.
  5. 5. according to a kind of 3D printing glass powder, preparation method thereof described in claim 1, it is characterised in that：The step (5) will Sieved to obtain safety glass powder with 400 mesh sieve after glass breaking, grinding.
  6. 6. according to a kind of 3D printing glass powder, preparation method thereof described in claim 1, it is characterised in that：The step (6) is right Mixed powder is ground, and the grinding is carried out using ball milling method.
  7. 7. according to a kind of 3D printing glass powder, preparation method thereof described in claim 6, it is characterised in that：Step (6) ball The condition of mill is：The mass ratio of big ball and bead is 2：The mass ratio of 1.3-1.5, abrading-ball and material is 10：0.8-1.2, rotating speed For 600-1200rpm, Ball-milling Time 25-35min.
CN201710646902.6A 2017-08-01 2017-08-01 A kind of 3D printing glass powder, preparation method thereof Pending CN107417127A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110078373A (en) * 2019-05-14 2019-08-02 山东硼硅玻璃制品有限公司 A kind of preparation method of medical 3: 3 high boron-silicon glass pipe material
CN113415999A (en) * 2021-05-25 2021-09-21 赵凤宇 Micro glass metal 3D printing micro powder for liquid printer

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271783A (en) * 2015-10-21 2016-01-27 武汉理工大学 Glass powder for 3D (three dimensional) printing and preparation method of glass powder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271783A (en) * 2015-10-21 2016-01-27 武汉理工大学 Glass powder for 3D (three dimensional) printing and preparation method of glass powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110078373A (en) * 2019-05-14 2019-08-02 山东硼硅玻璃制品有限公司 A kind of preparation method of medical 3: 3 high boron-silicon glass pipe material
CN113415999A (en) * 2021-05-25 2021-09-21 赵凤宇 Micro glass metal 3D printing micro powder for liquid printer

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