CN105113002B - A kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation - Google Patents
A kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation Download PDFInfo
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Abstract
The present invention is a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation, is characterized in：Comprise the following steps：Feature carbon felt is pre-processed；Prepare epoxy resin adhesive and phenolic resin adhesive；It is prepared by the prepreg of feature carbon felt；It is prepared by mold；Clipping function carbon felt；Make guide shell precast body；Resin solidification and resin carbonation processing；Machining；It is prepared by face coat." falling pot " phenomenon of conventional graphite guide shell can be thoroughly solved using the present invention；Once mounting in place, without repeated disassembled and assembled；Thermal field heat is reduced to scatter and disappear and operation power；Improve pulling rate and crystal bar yield rate；Improve heat endurance, anti-air-flow and the particulate matter performance of flushing on guide shell surface.With reducing, thermal field heat is lost, mitigate guide shell weight, increases the advantage of guide shell surface strength.
Description
Technical field
The invention belongs to photovoltaic field, it is related to a kind of preparation method of monocrystalline silicon growing furnace guide shell, especially relates to
And a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation.
Background technology
Guide shell is one of indispensable insulation device in current monocrystalline silicon growing furnace thermal field, positioned at the upper of molten silica crucible liquid level
Side, its main function includes：Orientation is guided air-flow；Increase longitudinal temperature gradient, improve crystal bar pulling rate；Reduce heat energy loss,
Reduction operation power.Conventional guide shell is a kind of high-purity, isostatic pressing formed graphite device, is had the disadvantage：
1. because graphite material thermal conductivity is higher, cause the lost very fast, heat insulation effect of heat of thermal field poor；Then make
Longitudinal temperature gradient in thermal field does not reach due difference, or scatters and disappears into the heat around crystal boundary face uneven, causes crystal bar
There is bird caging phenomenon, these situations can all directly affect the normal growth of silicon crystal, reduce the yield rate of crystal bar.In order to change
This defect of kind graphite guide shell, Normal practice is the operation power for increasing thermal field, and this heat energy that certainly will aggravate whole system disappears
Consumption；
2. conventional graphite guide shell is combined by inside and outside two layers of cylinder, sometimes middle to be also filled with insulation material,
Therefore not only weight is larger, and also needs to often change insulation filler, is both not easy to dismounting, can occur in use again
" falling pot " phenomenon, causes whole pot material scrap, damages the even whole thermal field of crucible, heater；
3. under the souring of particulate matter, silicon steam and oxidizing gas, conventional guide shell is in short-period used
Afterwards, surface is also easy to produce the phenomenons such as burn into cracking and chip off-falling, so as to significantly shorten its service life.
The content of the invention
The purpose of the present invention is：A kind of monocrystalline silicon growing furnace guide shell preparation side of feature carbon felt global formation is provided
Method, can reduce thermal field heat and scatter and disappear, mitigate guide shell weight, increase guide shell surface strength.
The present invention is realized by following technical scheme：A kind of monocrystalline silicon growing furnace of feature carbon felt global formation is led
Flow cartridge preparation method, it is characterized in that：Using feature carbon felt as raw material global formation guide shell；And use carbon/carbon composite mortar
Paint-on technique makes guide shell face coat, specifically includes following steps：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of h of drying in oven 1 ~ 8；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
3）Prepared by the prepreg of feature carbon felt, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of h of drying in oven 9 ~ 18 afterwards；Carbon felt surface uniform coating step 2 again）Obtained phenolic resin gluing
Agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Mold preparation, the concrete shape required according to product drawing, size, processing prepares corresponding mold；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 4 ~ 9 layer function carbon felt Prepreg Lays, coat simultaneously
Guide shell mold outer surface is fixed on, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, and solidification 10 ~
20 h, obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 10 ~ 25h at 1000 DEG C；Again
In 15 ~ 40h of high temperature cabonization at 2000 DEG C, guide shell precast body III is obtained；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic aldehyde tree
Fat B：Solvent B=1：（2~3）：（5~6）And each raw material is mixed, stirred；Gained carbon/carbon composite mortar is uniformly coated
In the surface of guide shell precast body III, the mm of coat thickness 0.2~1.5；It is then fed into curing oven, 15 is carried out at 220 DEG C
~24h baking processing；It is sent to again in carbide furnace, in the 10~30h that is carbonized at 1200 DEG C, obtains guide shell precast body IV；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Bakelite B：
Solvent B=1：（2~3）：（5~6）And each raw material is mixed, stirred；Gained composite mortar is evenly applied to guide shell pre-
The surface of body IV processed, 0.2~1.5mm of coat thickness；It is then fed into curing oven, 15~24 h baking is carried out at 220 DEG C
Roasting processing；It is sent to again in carbide furnace, in the 10~30h that at 1800 DEG C, is carbonized, obtains guide shell precast body V；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Bakelite B：
Solvent B=1：（2~3）：（5~6）And each raw material is mixed, stirred；Gained slurry is evenly applied to guide shell precast body
V surface, 0.2~1.5mm of coat thickness；It is then fed into curing oven, at the baking that 15~24 h are carried out at 220 DEG C
Reason；It is sent to again in carbide furnace, it is final to obtain guide shell product in the 10~30h that at 1800 DEG C, is carbonized.
The step 2）In epoxy resin A be epoxy resin E-56D.
The step 2）In epoxy resin B be epoxy resin E-51.
The step 2）In solvent orange 2 A be ethanol.
The step 2）In phenol-formaldehyde A be 6812 thermoplastic phenolic resins.
The step 2）In curing agent be hexa.
The step 2）、10）、11）、12）In solvent B be acetone.
The step 10）、12）In reinforcing agent A be boron carbide powder, wherein step 10）The granularity of boron carbide powder used is
325 mesh, step 12）The granularity of boron carbide powder used is 500 mesh.
The step 10）、11）、12）In bakelite B be HK-2506 type thermosetting phenolic resins.
The step 11）In reinforcing agent B be CQ-300 fume colloidal silicas.
The beneficial effects of the invention are as follows：
Few, the high insulating effect 1. thermal field heat scatters and disappears, runs power low；Pulling rate is improved, crystal bar yield rate is significantly carried
Rise；
2. monolithic devices guide shell is lightweight；Only need once mounting in place, without traditional dismounting process process, thoroughly solve
Phenomenon of certainly " falling pot "；
3. guide shell surface strength is high, thermally-stabilised good, the better performances that anti-air-flow and particulate matter are washed away.
Embodiment
With reference to embodiment, the present invention is further described.
A kind of embodiment 1, the monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation is specific to make
Step is as follows：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of h of drying in oven 1；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
The epoxy resin A is epoxy resin E-56D, and epoxy resin B is epoxy resin E-51, and solvent orange 2 A is ethanol, phenolic aldehyde
Resin A is 6812 thermoplastic phenolic resins, and curing agent is hexa, and solvent B is acetone；
3）Prepared by feature carbon felt prepreg, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of drying in oven 9h afterwards；Feature Carbon felt surface uniform coating step 2 again）Obtained phenolic resin gluing
Agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Prepared by mold, corresponding mold is prepared according to shape of product size design；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 4 layer function carbon felt Prepreg Lays, cladding and fixation
In guide shell mold outer surface, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 10 h, obtains
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 10 h at 1000 DEG C；Then at
The h of high temperature cabonization 15 at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic aldehyde
Resin B：Solvent B=1：2：5~6 and by each raw material mix, stir；Gained carbon/carbon composite mortar is evenly applied to water conservancy diversion
The surface of cylinder precast body III, the mm of coat thickness 0.20；It is then fed into curing oven, at the baking that 15h is carried out at 220 DEG C
Reason；It is sent to again in carbide furnace, in 10 h that are carbonized at 1200 DEG C, obtains guide shell precast body IV；
The reinforcing agent A is the boron carbide powder of 325 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Bakelite B：
Solvent B=1：2：5 and by each raw material mix, stir；Gained slurry is evenly applied to the surface of guide shell precast body IV,
Coat thickness 0.20mm；It is then fed into curing oven, 15h baking processing is carried out at 220 DEG C；Carbide furnace is sent to again
In, in the 10h that at 1800 DEG C, is carbonized, obtain guide shell precast body V；
The reinforcing agent B is CQ-300 fume colloidal silicas, and bakelite B is HK-2506 type thermosetting phenolic resins, molten
Agent B is acetone；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic resin
B：Solvent B=1：2：5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body V
Surface, coat thickness 0.2mm；It is then fed into curing oven, 15h baking processing is carried out at 220 DEG C；Carbon is sent to again
Change in stove, it is final to obtain guide shell product in the 10h that at 1800 DEG C, is carbonized.
The reinforcing agent A is the boron carbide powder of 500 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone.
Embodiment 2, the specific making step of the present embodiment is as follows：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of h of drying in oven 3；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
The epoxy resin A is epoxy resin E-56D, and epoxy resin B is epoxy resin E-51, and solvent orange 2 A is ethanol, phenolic aldehyde
Resin A is 6812 thermoplastic phenolic resins, and curing agent is hexa, and solvent B is acetone；
3）Prepared by feature carbon felt prepreg, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of h of drying in oven 11 afterwards；Feature Carbon felt surface uniform coating step 2 again）Obtained phenolic resin glue
Glutinous agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Prepared by mold, corresponding mold is prepared according to shape of product size design；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 5 layer function carbon felt Prepreg Lays, coat and be fixed on
Guide shell mold outer surface, obtains guide shell precast body I；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 11 h, obtains
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 13h at 1000 DEG C；Then at
High temperature cabonization 20h at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic aldehyde tree
Fat B：Solvent B=1：2.5：5 and by each raw material mix, stir；Gained carbon/carbon composite mortar is evenly applied to guide shell
The surface of precast body III, coat thickness 0.46mm；It is then fed into curing oven, 17h baking processing is carried out at 220 DEG C；
It is sent to again in carbide furnace, in the 14h that is carbonized at 1200 DEG C, obtains guide shell precast body IV；
The reinforcing agent A is the boron carbide powder of 325 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Phenolic resin
B：Solvent B=1：2.5：5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body IV
Surface, coat thickness 0.46mm；It is then fed into curing oven, 17h baking processing is carried out at 220 DEG C；Sent again
Enter in carbide furnace, in the 14h that at 1800 DEG C, is carbonized, obtain guide shell precast body V；
The reinforcing agent B is CQ-300 fume colloidal silicas, and bakelite B is HK-2506 type thermosetting phenolic resins, molten
Agent B is acetone；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Bakelite B：
Solvent B=1：2.5：5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body V
Surface, coat thickness 0.45mm；It is then fed into curing oven, 17h baking processing is carried out at 220 DEG C；It is sent to again
It is final to obtain guide shell product in the 14h that at 1800 DEG C, is carbonized in carbide furnace.
The reinforcing agent A is the boron carbide powder of 500 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone.
Embodiment 3, the specific making step of the present embodiment is as follows：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of drying in oven 4h；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
The epoxy resin A is epoxy resin E-56D, and epoxy resin B is epoxy resin E-51, and solvent orange 2 A is ethanol, phenolic aldehyde
Resin A is 6812 thermoplastic phenolic resins, and curing agent is hexa, and solvent B is acetone；
3）Prepared by feature carbon felt prepreg, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of drying in oven 13h afterwards；Feature Carbon felt surface uniform coating step 2 again）Obtained phenolic resin glue
Glutinous agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Prepared by mold, corresponding mold is prepared according to shape of product size design；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 6 layer function carbon felt Prepreg Lays, cladding and fixation
In guide shell mold outer surface, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 14 h,
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 16h at 1000 DEG C；Then at
High temperature cabonization 25h at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic aldehyde
Resin B：Solvent B=1：3：5 and by each raw material mix, stir；Gained carbon/carbon composite mortar is evenly applied to guide shell
The surface of precast body III, coat thickness 0.72mm；It is then fed into curing oven, 19h baking processing is carried out at 220 DEG C；
It is sent to again in carbide furnace, in the 18h that is carbonized at 1200 DEG C, obtains guide shell precast body IV；
The reinforcing agent A is the boron carbide powder of 325 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Phenolic resin
B：Solvent B=1：3：5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body IV
Surface, coat thickness 0.72mm；It is then fed into curing oven, 19h baking processing is carried out at 220 DEG C；It is sent to again
In carbide furnace, in the 18h that at 1800 DEG C, is carbonized, guide shell precast body V is obtained；
The reinforcing agent B is CQ-300 fume colloidal silicas, and bakelite B is HK-2506 type thermosetting phenolic resins, molten
Agent B is acetone；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic resin
B：Solvent B=1：3：5 and by each raw material mix, stir；Gained slurry is evenly applied to the table of guide shell precast body V
Face, coat thickness 0.72mm；It is then fed into curing oven, 19h baking processing is carried out at 220 DEG C；Carbon is sent to again
Change in stove, it is final to obtain guide shell product in the 18h that at 1800 DEG C, is carbonized.
The reinforcing agent A is the boron carbide powder of 500 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone.
Embodiment 4, the specific making step of the present embodiment is as follows：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of drying in oven 6h；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
The epoxy resin A is epoxy resin E-56D, and epoxy resin B is epoxy resin E-51, and solvent orange 2 A is ethanol, phenolic aldehyde
Resin A is 6812 thermoplastic phenolic resins, and curing agent is hexa, and solvent B is acetone；
3）Prepared by feature carbon felt prepreg, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of drying in oven 14h afterwards；Feature Carbon felt surface uniform coating step 2 again）Obtained phenolic resin glue
Glutinous agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Prepared by mold, corresponding mold is prepared according to shape of product size design；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 7 layer function carbon felt Prepreg Lays, cladding and fixation
In guide shell mold outer surface, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 16h, obtains
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 19h at 1000 DEG C；Then at
High temperature cabonization 30h at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10. prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, its mass ratio is reinforcing agent A：Phenolic aldehyde
Resin B：Solvent B=1：3：5.5 and by each raw material mix, stir；Gained carbon/carbon composite mortar is evenly applied to water conservancy diversion
The surface of cylinder precast body III, coat thickness 0.98mm；It is then fed into curing oven, at the baking that 21h is carried out at 220 DEG C
Reason；It is sent to again in carbide furnace, in the 22h that is carbonized at 1200 DEG C, obtains guide shell precast body IV；
The reinforcing agent A is the boron carbide powder of 325 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Phenolic resin
B：Solvent B=1：3：5.5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body IV
Surface, coat thickness 0.98mm；It is then fed into curing oven, 21h baking processing is carried out at 220 DEG C；Sent again
Enter in carbide furnace, in the 22h that at 1800 DEG C, is carbonized, obtain guide shell precast body V；
The reinforcing agent B is CQ-300 fume colloidal silicas, and bakelite B is HK-2506 type thermosetting phenolic resins, molten
Agent B is acetone；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic resin
B：Solvent B=1：3：5.5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body V
Surface, coat thickness 0.98mm；It is then fed into curing oven, 21h baking processing is carried out at 220 DEG C；Sent again
Enter in carbide furnace, it is final to obtain guide shell product in the 22h that at 1800 DEG C, is carbonized.
The reinforcing agent A is the boron carbide powder of 500 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone.
Embodiment 5, the specific making step of the present embodiment is as follows：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of drying in oven 7h；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
The epoxy resin A is epoxy resin E-56D, and epoxy resin B is epoxy resin E-51, and solvent orange 2 A is ethanol, phenolic aldehyde
Resin A is 6812 thermoplastic phenolic resins, and curing agent is hexa, and solvent B is acetone；
3）Prepared by feature carbon felt prepreg, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of drying in oven 16h afterwards；Feature Carbon felt surface uniform coating step 2 again）Obtained phenolic resin glue
Glutinous agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Prepared by mold, corresponding mold is prepared according to shape of product size design；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 8 layer function carbon felt Prepreg Lays, cladding and fixation
In guide shell mold outer surface, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 18h, obtains
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 22h at 1000 DEG C；Then at
High temperature cabonization 35h at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic aldehyde tree
Fat B：Solvent B=1：3：6 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body III
Surface, coat thickness 1.24mm；It is then fed into curing oven, 23h baking processing is carried out at 220 DEG C；Sent again
Enter in carbide furnace, in the 26h that is carbonized at 1200 DEG C, obtain guide shell precast body IV；
The reinforcing agent A is the boron carbide powder of 325 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Bakelite B：
Solvent B=1：3：6 and by each raw material mix, stir；Gained composite mortar is evenly applied to the table of guide shell precast body IV
Face, coat thickness 1.24mm；It is then fed into curing oven, 23h baking processing is carried out at 220 DEG C；Carbon is sent to again
Change in stove, in the 26h that at 1800 DEG C, is carbonized, obtain guide shell precast body V；
The reinforcing agent B is CQ-300 fume colloidal silicas, and bakelite B is HK-2506 type thermosetting phenolic resins, molten
Agent B is acetone；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic resin
B：Solvent B=1：3：6 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body V
Surface, coat thickness 1.24mm；It is then fed into curing oven, 23h baking processing is carried out at 220 DEG C；It is sent to again
It is final to obtain guide shell product in the 26h that at 1800 DEG C, is carbonized in carbide furnace.
The reinforcing agent A is the boron carbide powder of 500 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone.
Embodiment 6, the specific make step of the present embodiment is as follows：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of drying in oven 8h；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy are prepared respectively according to quality proportioning
The mass ratio of Resin adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is
Phenol-formaldehyde A：Curing agent：Solvent B=7：0.5：3；
The epoxy resin A is epoxy resin E-56D, and epoxy resin B is epoxy resin E-51, and solvent orange 2 A is ethanol, phenolic aldehyde
Resin A is 6812 thermoplastic phenolic resins, and curing agent is hexa, and solvent B is acetone；
3）Prepared by feature carbon felt prepreg, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin gluing
Agent, sends into 180 DEG C of drying in oven 18h afterwards；Feature Carbon felt surface uniform coating step 2 again）Obtained phenolic resin glue
Glutinous agent, stands 24 h in dry environment, and volatilize the volatile matters such as moisture, solvent and free phenol；
4）Prepared by mold, corresponding mold is prepared according to shape of product size design；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 9 layer function carbon felt Prepreg Lays, cladding and fixation
In guide shell mold outer surface, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 20h, obtains
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 25h at 1000 DEG C；Then at
High temperature cabonization 40h at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, outer to ensure
Shape is of the required size；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic aldehyde
Resin B：Solvent B=1：2.5：5.5 and by each raw material mix, stir；Gained carbon/carbon composite mortar is evenly applied to lead
The surface of flow cartridge precast body III, coat thickness 1.50mm；It is then fed into curing oven, at the baking that 24h is carried out at 220 DEG C
Reason；It is sent to again in carbide furnace, in 30 h that are carbonized at 1200 DEG C, obtains guide shell precast body IV；
The reinforcing agent A is the boron carbide powder of 325 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Phenolic resin
B：Solvent B=1：2.5：5.5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body
IV surface, coat thickness 1.50mm；It is then fed into curing oven, 24h baking processing is carried out at 220 DEG C；Again by it
Send into carbide furnace, in the 30h that at 1800 DEG C, is carbonized, obtain guide shell precast body V；
The reinforcing agent B is CQ-300 fume colloidal silicas, and bakelite B is HK-2506 type thermosetting phenolic resins, molten
Agent B is acetone；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Phenolic resin
B：Solvent B=1：2.5：5.5 and by each raw material mix, stir；Gained composite mortar is evenly applied to guide shell precast body
V surface, coat thickness 1.50mm；It is then fed into curing oven, 24h baking processing is carried out at 220 DEG C；Again by it
Send into carbide furnace, it is final to obtain guide shell product in the 30h that at 1800 DEG C, is carbonized.
The reinforcing agent A is the boron carbide powder of 500 mesh, and bakelite B is HK-2506 type thermosetting phenolic resins, solvent B
For acetone.
Claims (10)
1. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation, it is characterized in that：With Functional carbon
Felt is raw material global formation guide shell；And guide shell face coat, specific bag are made using carbon/carbon composite mortar paint-on technique
Include following steps：
1）Feature carbon felt is pre-processed, by feature carbon felt in 100 DEG C of h of drying in oven 1 ~ 8；
2）Adhesive is prepared, epoxy resin adhesive and phenolic resin adhesive, epoxy resin are prepared respectively according to quality proportioning
The mass ratio of adhesive is epoxy resin A：Epoxy resin B：Solvent orange 2 A=1：3：2, the mass ratio of phenolic resin adhesive is phenolic aldehyde
Resin A：Curing agent：Solvent B=7：0.5：3；
3）Prepared by the prepreg of feature carbon felt, feature carbon felt is sufficiently impregnated step 2）Obtained epoxy resin adhesive,
180 DEG C of h of drying in oven 9 ~ 18 are sent into afterwards；Carbon felt surface uniform coating step 2 again）Obtained phenolic resin adhesive,
24 h, the volatile matter of volatilization moisture, solvent and free phenol are stood in dry environment；
4）Mold preparation, the concrete shape required according to product drawing, size, processing prepares corresponding mold；
5）Clipping function carbon felt, the shape and size clipping function carbon felt according to guide shell mold；
6）Guide shell precast body is made, by step 5）Obtained 4 ~ 9 layer function carbon felt Prepreg Lays, cladding and fixation
In guide shell mold outer surface, guide shell precast body I is obtained；
7）Resin solidification processing, sends guide shell precast body I into baking oven, under the conditions of 160 DEG C, 5MPa, solidifies 10 ~ 20 h,
Obtain guide shell precast body II；
8）Resin carbonation processing, sends guide shell precast body II into carbide furnace, and be first carbonized 10 ~ 25h at 1000 DEG C；Then at
15 ~ 40h of high temperature cabonization at 2000 DEG C, obtains guide shell precast body III；
9）Machining, is machined to the guide shell precast body III obtained by above-mentioned steps, to ensure profile chi
It is very little to meet the requirements；
10）Prepared by face coat I, carbon/carbon composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Bakelite B：
Solvent B=1：（2~3）：（5~6）And each raw material is mixed, stirred；Gained carbon/carbon composite mortar is evenly applied to lead
The surface of flow cartridge precast body III, the mm of coat thickness 0.2~1.5；Be then fed into curing oven, at 220 DEG C carry out 15~
24h baking processing；It is sent to again in carbide furnace, in the 10~30h that is carbonized at 1200 DEG C, obtains guide shell precast body IV；
11）Prepared by face coat II, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent B：Bakelite B：Solvent
B=1：（2~3）：（5~6）And each raw material is mixed, stirred；Gained composite mortar is evenly applied to guide shell precast body
IV surface, 0.2~1.5mm of coat thickness；It is then fed into curing oven, at the baking that 15~24 h are carried out at 220 DEG C
Reason；It is sent to again in carbide furnace, in the 10~30h that at 1800 DEG C, is carbonized, obtains guide shell precast body V；
12）Prepared by face coat III, composite mortar is obtained by quality proportioning, and its mass ratio is reinforcing agent A：Bakelite B：Solvent
B=1：（2~3）：（5~6）And each raw material is mixed, stirred；Gained slurry is evenly applied to guide shell precast body V
Surface, 0.2~1.5mm of coat thickness；It is then fed into curing oven, 15~24 h baking processing is carried out at 220 DEG C；Again
It is sent in carbide furnace, it is final to obtain guide shell product in the 10~30h that at 1800 DEG C, is carbonized.
2. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 2）In epoxy resin A be epoxy resin E-56D.
3. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 2）In epoxy resin B be epoxy resin E-51.
4. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 2）In solvent orange 2 A be ethanol.
5. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 2）In phenol-formaldehyde A be 6812 thermoplastic phenolic resins.
6. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 2）In curing agent be hexa.
7. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 2）、10）、11）、12）In solvent B be acetone.
8. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 10）、12）In reinforcing agent A be boron carbide powder, wherein step 10）The granularity of boron carbide powder used is
325 mesh, step 12）The granularity of boron carbide powder used is 500 mesh.
9. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation as claimed in claim 1, its
It is characterized in：The step 10）、11）、12）In bakelite B be HK-2506 type thermosetting phenolic resins.
10. a kind of monocrystalline silicon growing furnace guide shell preparation method of feature carbon felt global formation described in claim 1, it is special
Levying is：The step 11）In reinforcing agent B be CQ-300 fume colloidal silicas.
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| CN109824373A (en) * | 2019-03-08 | 2019-05-31 | 佛山市石金科技有限公司 | A kind of preparation method of functionality heat-preservation cylinder felt |
| CN114671699A (en) * | 2022-04-29 | 2022-06-28 | 吉林联科特种石墨材料有限公司 | Preparation method of carbon fiber cylindrical high-temperature heat insulation material with integrated functions |
| CN114773080A (en) * | 2022-05-10 | 2022-07-22 | 吉林联科特种石墨材料有限公司 | Preparation method of three-in-one heat-insulating material with graphene as heat reflecting layer |
| CN114907144B (en) * | 2022-06-06 | 2023-04-18 | 吉林联科特种石墨材料有限公司 | Method for preparing SiC-C composite high-temperature coating by one-step method |
| CN114920573A (en) * | 2022-06-06 | 2022-08-19 | 吉林联科特种石墨材料有限公司 | Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material |
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| JPH05294779A (en) * | 1992-04-23 | 1993-11-09 | Kawasaki Steel Corp | Single crystal pulling up device |
| CN100400471C (en) * | 2006-07-20 | 2008-07-09 | 西安超码科技有限公司 | Method for manufacture thermal field charcoal/charcoal draft tube for single crystal silicon pulling furnace |
| JP4919343B2 (en) * | 2007-02-06 | 2012-04-18 | コバレントマテリアル株式会社 | Single crystal pulling device |
| CN100595350C (en) * | 2008-03-03 | 2010-03-24 | 湖南金博复合材料科技有限公司 | Single-crystal furnace guide shell and production process thereof |
| CN101948327B (en) * | 2010-08-17 | 2012-12-12 | 西安超码科技有限公司 | Method for preparing work hardening insulation quilt for high temperature furnace |
| CN101949481B (en) * | 2010-09-17 | 2011-12-14 | 西安超码科技有限公司 | Method for preparing wound heat-insulating drum |
| CN102010231B (en) * | 2010-10-24 | 2013-05-22 | 西安超码科技有限公司 | Method for preparing low-density carbon/carbon composite material surface coating |
| CN103183518A (en) * | 2011-12-27 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Method for preparing carbon/carbon composite material draft tube |
| CN102912425B (en) * | 2012-10-22 | 2015-06-17 | 湖南金博复合材料科技有限公司 | Guide cylinder and preparation method thereof |
| CN104891950B (en) * | 2015-05-12 | 2017-04-05 | 湖南搏盛天弘新材料技术有限公司 | A kind of hard carbon fibre thermal-insulation plate and preparation method thereof |
| CN104911696A (en) * | 2015-06-30 | 2015-09-16 | 湖南南方搏云新材料有限责任公司 | Immobilized-carbon felt overall draft tube for Czochralski silicon single crystal furnace and preparation method of draft tube |
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