CN1252399C - Nanometer ceramic spring producing method - Google Patents
Nanometer ceramic spring producing method Download PDFInfo
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- CN1252399C CN1252399C CN 03132051 CN03132051A CN1252399C CN 1252399 C CN1252399 C CN 1252399C CN 03132051 CN03132051 CN 03132051 CN 03132051 A CN03132051 A CN 03132051A CN 1252399 C CN1252399 C CN 1252399C
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- base substrate
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Abstract
The present invention provides a nanometer ceramic spring production method which is characterized in that nanometer ZrO2 powder is used as raw materials; pre-mixed liquid is added to the raw materials; the mixture is ground and mixed in a ball mill for slurry preparation; the prepared slurry is processed by vacuum deaeration, and then evocating agents are added to the prepared slurry; the mixed slurry is injected in a spring mould; the mixed slurry after solidification is demoulded and dried for 0.5 to 3 hours at 50 DEG C to 120 DEG C to obtain a spring body; the dry spring body is heated to 700 DEG C to 1200 DEG C, and thermal insulationfor lasts for 0.5 to 2 hours; then, adhesives are removed; the spring body after the adhesives are removed is processed by dipping gum; in the environment of normal pressure or vacuum, the body is put in slurry of which the concentration is from 30 wt% to 70 wt% for dipping gum 10 to 30 minutes; the compact spring body after dipping gum is put in a supporter and a powder bed; the spring body is put in a nodulize furnace to be heated to 1400 DEG to 1700 DEGC, and thermal insulation lasts for 0.5 to 3 hours for unpressurized nodulize to obtain a finished product. The present invention has the advantages of low cost, stable product quality and high reliability. The present invention which is suitable for mass production, can meet the needs of practicality.
Description
Technical field
The present invention relates to a kind of production method of nonmetal spring, specifically a kind of nano ceramics spring production method.
Background technique
Spiral spring is the elastic part of using always, and is extremely wide in various application in machine equipments, adopt metallic material to roll usually and form, but the poor-performing such as heat-resisting, anti-corrosion and wear-resisting of metal spring.By contrast, excellent properties such as it is high temperature resistant, corrosion-resistant, wear-resistant that stupalith has be used widely in each field, but because pottery is a kind of brittle material, the past can't directly be made spring always.But along with the development of nano-fabrication technique and high-performance ceramic technology, some have the nano ceramic such as the zirconium oxide (ZrO of higher toughness
2), silicon nitride (Si
3N
4) be developed, and obtained utilization widely in mechanical industry, make that utilizing pottery to make spring as raw material becomes possibility.Because the utilization of ceramics springs has a extensive future, so major industrial countries such as present America and Japan are being devoted to the development of ceramics springs, but all is in laboratory stage, the manufacture cost height, complex process can't be produced ceramics springs in batches to satisfy growing demand.And product is because defective such as hole, and quality instability, poor reliability are difficult to satisfy practical requirement.
Summary of the invention
The purpose of this invention is to provide a kind of with nanometer ZrO
2Industrialized preparing process for the ceramics springs of raw material.
Technological scheme of the present invention is:
A kind of nano ceramics spring production method is provided, it is characterized in that: with nanometer ZrO
2Powder is a raw material, and its production method is: the slip preparation → notes type → demoulding drying → binder removal → soaking paste → sintering → finished product that congeals into.
(a) slip preparation: with nanometer ZrO
2Powder is a raw material, adds premixed liquid and carry out ground and mixed preparation slip in pebble mill;
(b) annotate the type that congeals into: the slip for preparing is carried out adding initator after the vacuum outgas moulding in the floating die assembly that reinjects;
(c) demoulding drying: treat the slip curing and demolding, put into baking oven and be heated to 50 ℃～120 ℃ dryings 0.5～3 hour, and natural cooling, obtain the spring base substrate;
(d) binder removal: the spring base substrate behind the natural cooling is heated to 700 ℃～1200 ℃ in electric furnace of resistance type, and is incubated 0.5～3 hour, carry out binder removal, and natural cooling;
(e) soaking paste: the spring base substrate behind binder removal and the natural cooling is carried out soaking paste, in normal pressure or vacuum environment, is soaking paste 10～30 minutes in the slip of 30wt%～70wt% with base substrate in concentration;
(f) sintering: the spring base substrate after the soaking paste densification is placed support and bury powder, put into sintering furnace and be heated to 1400 ℃～1700 ℃, and be incubated 0.5～3 hour and do not have pressure, obtain finished product around knot.
The premixed liquid that uses in the slurry process for preparation is made up of water, dispersing agent and organic monomer; The effect of dispersing agent is that inorganic ceramic powder and organic principle in the slurry are evenly mixed, prevent to reunite, improve solid content of slurry and flowability, dispersing agent commonly used is: a kind of or wherein several combination in polyacrylic acid and salt thereof, polymethacrylic acid and salt thereof, polyvinyl-pyrrolidone (PVP), polyacrylamide, the lignosulfonates.Organic monomer is the material base that forms polymer, when using water as solvent, organic monomer should satisfy: must be water miscible, the gel that is formed by monomer solution should have certain intensity, not influence the flowability of slurry, and organic monomer commonly used is: a kind of or wherein several combination in NMA (HMAM), acrylamide (AM), acrylic acid, Methacrylamide (MAM), methacrylic acid, methoxy poly (ethylene glycol) monomethyl propylene ester (MPEGMA), the n-vinyl pyrrolidone (n-NVP).
The congeal into thinking of type of notes is the concentrate suspension slip of the high solid volume fraction of low viscosity that will preparation, under action of evocating, makes the organic monomer cross-linked polymeric in the suspension become tridimensional network, thereby makes the moulding of suspension in-situ solidifying.The slip for preparing is added initator through after the vacuum outgas, inject floating die assembly, treat the slip curing and demolding.Initator is used for causing polymerisation, a kind of or wherein several combination in the mixture of mixture, potassium peroxydisulfate, potassium peroxydisulfate and tetramethylethylenediamine that ammonium persulphate (APS), ammonium persulphate and tetramethylethylenediamine are arranged commonly used.
Treat the slip curing and demolding, put into baking oven and be heated to 50 ℃～120 ℃ dryings 0.5～3 hour, and natural cooling, the spring base substrate obtained;
The binder removal process is that base substrate is heated to 700 ℃～1200 ℃, and is incubated 0.5～3 hour, discharges organic principle.
Spring base substrate behind binder removal and the natural cooling is carried out soaking paste, in normal pressure or vacuum environment, is soaking paste 10～30 minutes in the slip of 30wt%～70wt% with base substrate in concentration, to eliminate the pore that causes because of binder removal in the base substrate.If the spring base substrate without binder removal and soaking paste step, will stay a lot of pores after organic principle is excluded when sintering, influence the quality of final products.The present invention just can avoid this generation of defects with the spring base substrate through carrying out the soaking paste densification again after the binder removal operation.
Spring base substrate after the soaking paste densification is placed support and bury powder, put into sintering furnace and be heated to 1400 ℃～1700 ℃ in three stages, and be incubated 0.5～3 hour and do not have pressure, obtain evenly neat ceramics springs finished product of profile after the cooling around knot.
Nano ceramics spring production method of the present invention also can adopt following method: batch mixing pugging → extrusion forming → drying → binder removal → soaking paste → sintering → finished product.
(a) batch mixing pugging: with nanometer ZrO
2Powder is a raw material, and the adding forming agent mixes stirring and obtains pug in pug mill;
(b) extrusion forming: pug is carried out extruding into wire rod after vacuum is mixed, and on spring coiling machine, roll into the spring base substrate;
(c) drying: the spring base substrate is put into baking oven and is heated to 50 ℃～120 ℃ and be incubated 0.5～3 hour together with supporting core, after the drying spring base substrate is taken off from core, carry out natural cooling;
(d) binder removal: natural cooling rear spring base substrate is heated to 700 ℃～1200 ℃ in electric furnace of resistance type, and is incubated 0.5～3 hour, carry out binder removal, carry out natural cooling behind the binder removal again;
(e) soaking paste: the spring base substrate behind binder removal and the natural cooling is carried out soaking paste, in normal pressure or vacuum environment, is soaking paste 10～30 minutes in the slip of 30wt%～70wt% with base substrate in concentration;
(f) sintering: the spring base substrate after the soaking paste densification is placed support and bury powder, put into sintering furnace and be heated to 1400 ℃～1700 ℃, and be incubated 0.5～3 hour and do not have pressure, obtain finished product after the cooling around knot.
The forming agent that adds in the batch mixing pugging comprises the mixture of methyl cellulose (MC), glycerine, water and polyvinyl alcohol (PVA) solution, the adding quantity of each composition of forming agent and the proportionate relationship of ceramic powder are: 100 parts of powders, 3～7 parts of methyl cellulose, 1～5 part of glycerine, 15～20 parts in water, 7～10 parts of poly-alcohol solutions.Methyl cellulose can play the effect that increases pug plasticity, makes it have the favorable mechanical performance, is beneficial to extrusion forming, the glycerine lubricate, prevent that pug is sticking glutinous, the mixture of poly-vinyl alcohol solution is a bond, makes the base substrate that extrudes out have certain intensity.
After mixing through vacuum again through the pug of batch mixing pugging, can extrude into wire rod, be around on the spring coiling machine, roll into spring, after the super-dry setting, take off again, carry out binder removal, soaking paste densification, sintering and obtain finished product from core.
Beneficial effect of the present invention:
1, solves the industrialized production difficult problem of ceramics springs, made the industrial applications of ceramics springs become possibility.
2, technology is succinct, and manufacturing equipment and raw material, auxiliary material are industrial chemicals commonly used, and cost is low.
3, product eliminates the surface pore defective, improved quality greatly, improved reliability.
4, employing dispersing agent and stabilizer have solved the powder particulate Stability Control problem in the ceramics springs production, adopt the composite forming technology of binder removal and soaking paste densification to solve the densification problem of complicated shape ceramic product, adopt support to add to bury the powder technology to have solved the problem on deformation of ceramics springs product in sintering process.
Embodiment
Embodiment one.
Get nanometer ZrO
2Powder 1000g, acrylamide 100g, ammonium polyacrylate 12.5g, water 1500g, ammonium persulfate aqueous solution (ammonium persulphate content 1%) 20g.With acrylamide 100g, ammonium polyacrylate 12.5g, water 1500g are mixed with premixed liquid and nanometer ZrO
2Powder 1000g obtains slip after adding the pebble mill mixing together, floating die assembly is injected in slime vacuum degassing back adding ammonium persulfate aqueous solution 20g mixing back treat the slip curing and demolding, put into baking oven then and be heated to 100 ℃, dry back natural cooling obtains the spring base substrate, the spring base substrate is put into electric furnace of resistance type be heated to 800 ℃ and be incubated 0.5 hour, carrying out binder removal handles, discharge organic component, treat to put into the slip that concentration is 50wt% behind its natural cooling, soaking paste is 10 minutes under vacuum environment, eliminate pore, at last the spring base substrate after the densification is placed supporting frame and bury powder and put into sintering furnace, obtain finished product 1600 ℃ of following pressureless sinterings 1 hour.
Embodiment two.
Get nanometer ZrO
2Powder 1000g, methyl cellulose 4wt%, glycerine 2wt%, water 15wt%, poly-vinyl alcohol solution (PVA content is 12wt%) 8wt%.After fully stirring pugging in powder and the forming agent adding vacuum pug mill, extrude into wire rod, roll into spring by spring coiling machine again, two ends are cut off in dry postboarding in 1 hour in 100 ℃ of baking ovens, obtain the spring base substrate, the about 2.5mm of spring filament diameter, the about 25mm of external diameter, the number of turns is 10 circles.In electric furnace of resistance type,, get rid of organic forming agent 800 ℃ of following biscuitings 0.5 hour.Carry out the soaking paste densification then under vacuum, pulp density is 50wt%, and the soaking paste time is 10 minutes.Base substrate after the densification 1600 ℃ of following pressureless sinterings 1 hour, is obtained finished product.The about 2mm of spring filament diameter of finished product, the about 25mm of external diameter, number of active coils are 10 circles.
Claims (7)
1, a kind of nano ceramics spring production method is characterized in that:
(a) with nanometer ZrO
2Powder is a raw material, and the adding premixed liquid carries out ground and mixed and carries out the slip preparation in pebble mill;
(b) slip for preparing is carried out adding initator after the vacuum outgas, in the floating die assembly that reinjects;
(c) treat the slip curing and demolding, in baking oven, be heated to 50 ℃～120 ℃ dryings 0.5～3 hour, and natural cooling, the spring base substrate obtained;
(d) the spring base substrate behind the natural cooling is heated to 700 ℃～1200 ℃ in electric furnace of resistance type, and is incubated 0.5～3 hour, carry out binder removal, and natural cooling;
(e) the spring base substrate behind binder removal and the natural cooling being carried out soaking paste, in normal pressure or vacuum environment, is soaking paste 10～30 minutes in the slip of 30wt%～70wt% with base substrate in concentration;
(f) the spring base substrate after the soaking paste densification is placed support and bury powder, put into sintering furnace and be heated to 1400 ℃～1700 ℃, and be incubated 0.5～3 hour and do not have pressure, obtain finished product around knot.
2, a kind of nano ceramics spring production method is characterized in that:
(a) with nanometer ZrO
2Powder is a raw material, and the adding forming agent mixes stirring and obtains pug in pug mill;
(b) pug is carried out extrude into wire rod after vacuum is mixed, and on spring coiling machine, roll into the spring base substrate;
(c) the spring base substrate is put into baking oven together with the support core and be heated to 50 ℃～120 ℃, and be incubated 0.5～3 hour, after the drying spring base substrate is taken off from core, carry out natural cooling;
(d) natural cooling rear spring base substrate is heated to 700 ℃～1200 ℃ in electric furnace of resistance type, and is incubated 0.5～3 hour, carry out binder removal, carry out natural cooling behind the binder removal again;
(e) the spring base substrate behind binder removal and the natural cooling being carried out soaking paste, in normal pressure or vacuum environment, is soaking paste 10～30 minutes in the slip of 30wt%～70wt% with base substrate in concentration;
(f) the spring base substrate after the soaking paste densification is placed support and bury powder, put into sintering furnace and be heated to 1400 ℃～1700 ℃, and be incubated 0.5～3 hour and do not have pressure, obtain finished product after the cooling around knot.
3, nano ceramics spring production method according to claim 1 is characterized in that described premixed liquid is made up of water, dispersing agent and organic monomer.
4, nano ceramics spring production method according to claim 1 is characterized in that described initator is a kind of or its combination in the mixture of mixture, potassium peroxydisulfate, potassium peroxydisulfate and tetramethylethylenediamine of ammonium persulphate, ammonium persulphate and tetramethylethylenediamine.
5, nano ceramics spring production method according to claim 3 is characterized in that described dispersing agent is a kind of or its combination in polyacrylic acid and salt, polymethacrylic acid and salt thereof, polyvinyl-pyrrolidone, polyacrylamide, the lignosulfonates.
6, nano ceramics spring production method according to claim 3 is characterized in that described organic monomer is a kind of or its combination in water miscible NMA, acrylamide, acrylic acid, Methacrylamide, methacrylic acid, methoxy poly (ethylene glycol), monomethyl propylene ester, the n-vinyl pyrrolidone.
7, nano ceramics spring production method according to claim 2, it is characterized in that described forming agent comprises the mixture of methyl cellulose, glycerine, water and poly-vinyl alcohol solution, the adding quantity of each composition of forming agent and the proportionate relationship of ceramic powder are: 100 parts of powders, 3～7 parts of methyl cellulose, 1～5 part of glycerine, 15～20 parts in water, 7～10 parts of poly-alcohol solutions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03132051 CN1252399C (en) | 2003-07-17 | 2003-07-17 | Nanometer ceramic spring producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03132051 CN1252399C (en) | 2003-07-17 | 2003-07-17 | Nanometer ceramic spring producing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1472448A CN1472448A (en) | 2004-02-04 |
| CN1252399C true CN1252399C (en) | 2006-04-19 |
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ID=34153964
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03132051 Expired - Fee Related CN1252399C (en) | 2003-07-17 | 2003-07-17 | Nanometer ceramic spring producing method |
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| CN (1) | CN1252399C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757221A (en) * | 2012-05-28 | 2012-10-31 | 南京工业大学 | Method for manufacturing spiral-shaped ceramic spring |
| CN103349918B (en) | 2013-06-19 | 2015-11-11 | 南京工业大学 | A kind of method preparing multichannel ceramic hollow fibrous membrane |
| CN106588000B (en) * | 2016-11-24 | 2020-11-10 | 上海交通大学 | Manufacturing process of spiral ceramic spring |
| CN109867526A (en) * | 2017-12-05 | 2019-06-11 | 辽宁法库陶瓷工程技术研究中心 | A kind of preparation method of refractory ceramics spring |
| CN110204313B (en) * | 2018-02-28 | 2021-10-15 | 清华大学 | Method for cross-linking and in-situ solidifying ceramic suspension by using dispersing agent and ceramic forming method |
| CN108679136B (en) * | 2018-05-18 | 2020-01-31 | 宁波市奇强精密冲件有限公司 | Spring holder of shock absorber |
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2003
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| CN1472448A (en) | 2004-02-04 |
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Granted publication date: 20060419 |